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Небесная энциклопедия

Космические корабли и станции, автоматические КА и методы их проектирования, бортовые комплексы управления, системы и средства жизнеобеспечения, особенности технологии производства ракетно-космических систем

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Мониторинг СМИ

Мониторинг СМИ и социальных сетей. Сканирование интернета, новостных сайтов, специализированных контентных площадок на базе мессенджеров. Гибкие настройки фильтров и первоначальных источников.

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Применить Всего найдено 5283. Отображено 100.

01-03-2012 дата публикации

Alkoxylated alkylamines/alkyl ether amines with peaked distribution

Номер: US20120053054A1

Автор: Alberto Slikta, David Becher, David Eaton, Giao Nguyen, Henry Agbaje, Kha Nguyen, Michael Seitz, Shawn Zhu

Принадлежит: Akzo Nobel NV

The present invention generally relates to a process for preparing the alkoxylated alkylamines and/or alkyl ether amines. The process consists of three stages, and utilizes an alkali catalyst. The alkoxylated alkyl amines and alkoxylated alkyl ether amines prepared by the process possess the peaked distribution and contain less hazardous by-product.

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Номер записи: 1

09-08-2012 дата публикации

Method for preparing polyamine compounds

Номер: US20120202934A1

Автор: Asghar Akber Peera, Glenn Nelson Robinson, Ian Anthony Tomlinson

Принадлежит: Angus Chemical Co, Dow Global Technologies LLC

A method for preparing a compound having formula (II) wherein R 1 and R 2 independently are methyl or ethyl, or R 1 and R 2 combine to form a C 5 or C 6 cycloalkyl or cycloalkenyl group. The method includes a step of combining R 1 R 2 CHNO 2 , glutaraldehyde and an amine. The compound is useful in coating compositions and other applications for pH adjustment.

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Номер записи: 2

18-10-2012 дата публикации

Process for preparing n,n-dimethylaminoethoxyethanol

Номер: US20120264979A1

Автор: Alfred Krause, Bernd Stein, Frank Haese, Frank-Friedrich Pape, Joachim-Thierry Anders, Johann-Peter Melder

Принадлежит: BASF SE

A process for preparing N,N-dimethylaminoethoxyethanol (DMAEE), wherein a) dimethylamine and ethylene oxide are reacted, b) the resulting product mixture of N,N-dimethylethanolamine and DMAEE is separated by distillation to obtain a DMAEE-containing fraction as the bottom stream, and c) DMAEE from the fraction obtained in (b) is removed by distillation.

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Номер записи: 3

21-02-2013 дата публикации

Method for the Hydrolysis of Substituted Formylamines into Substituted Amines

Номер: US20130046111A1

Автор: Mikhail Bobylev

Принадлежит: Individual

An improved method for the synthesis of substituted formylamines and substituted amines via an accelerated Leuckart reaction. The Leuckart reaction is accelerated by reacting formamide or N-alkylformamide and formic acid with an aldehyde or a ketone at a preferred molar ratio that accelerates the reaction. The improved method is applicable to various substituted aldehydes and ketones, including substituted benzaldehydes. An accelerated method for the hydrolysis of substituted formylamines into substituted amines using acid or base and a solvent at an elevated temperature. The improved method is useful for the accelerated synthesis of agrochemicals and pharmaceuticals such as vanillylamine, amphetamine and its analogs, and formamide fungicides.

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Номер записи: 4

04-04-2013 дата публикации

AROMATIC BUTAN-2-OL COMPOUNDS AND PREPARATION AND USES THEREOF

Номер: US20130085183A1

Автор: Li Song, Li Xingzhou, Liu Ping, Wang Lili, Wang Xiaokui, Xiao Junhai, Xie Yunde, Zhao Guoming, Zheng Zhibing, Zhong Wu, Zhou Xinbo

Принадлежит: INSTITUTE OF PHARMACOLOGY AND TOXICOLOGY ACADEMY OF MILITARY MEDICAL SCIENCES P.L.A. CHINA

Aromatic butan-2-ol compounds, preparation methods for making the compounds, and uses of the compounds are provided. Specifically, the compound of Formula I, or an optical isomer, racemate, diastereomer, pharmaceutically acceptable salt, or solvate thereof, is provided, where each of the substituents is defined. In addition, a pharmaceutical composition containing the compound, and the use of the compound in manufacture of a medicament for the treatment and/or prophylaxis of a disease or disorder caused by infection, is provided. 2. The compound of Formula I according to claim 1 , or an optical isomer claim 1 , racemate claim 1 , diastereomer claim 1 , pharmaceutically acceptable salt claim 1 , or solvate thereof claim 1 , wherein{'sub': '1', 'Rrepresents hydrogen, fluoro, chloro, bromo, iodo, or methoxy;'}{'sub': '2', 'Rrepresents hydrogen, fluoro, chloro, bromo, or iodo;'}{'sub': 3', '1-8, 'Rrepresents hydrogen, fluoro, chloro, bromo, iodo, or a Calkyl substituted at an o-, m-, or p-position of the phenyl ring;'}{'sub': '4', 'Rrepresents phenyl, substituted phenyl, or naphthyl; and'}{'sub': 5', '1-8, 'Rrepresents hydroxy, thiol, a Calkoxy, or methylthio.'}3. The compound of Formula I according to claim 2 , or an optical isomer claim 2 , racemate claim 2 , diastereomer claim 2 , pharmaceutically acceptable salt claim 2 , or solvate thereof claim 2 , wherein{'sub': '1', 'Rrepresents hydrogen, fluoro, chloro, bromo, or iodo;'}{'sub': 3', '1-6, 'Rrepresents hydrogen, fluoro, chloro, bromo, iodo, or a Calkyl substituted at an o-, m-, or p-position of the phenyl ring;'}{'sub': '4', 'Rrepresents phenyl, phenyl substituted with one or more halogens, or naphthyl; and'}{'sub': 5', '1-6, 'Rrepresents hydroxy or a Calkoxy.'}4. The compound of Formula I according to claim 3 , or an optical isomer claim 3 , racemate claim 3 , diastereomer claim 3 , pharmaceutically acceptable salt claim 3 , or solvate thereof claim 3 , wherein{'sub': '1', 'Rrepresents hydrogen, chloro, or bromo ...

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Номер записи: 5

04-04-2013 дата публикации

PROCESS FOR PRODUCING AN INTERMEDIATE FOR A CYCLIC CARBODIIMIDE COMPOUND

Номер: US20130085273A1

Автор: Shoji Shinichiro

Принадлежит: TEIJIN LIMITED

A process for producing an intermediate for a cyclic carbodiimide compound. 2. The production process according to claim 1 , wherein the metal catalyst is at least one selected from the group consisting of palladium claim 1 , ruthenium claim 1 , platinum claim 1 , rhodium claim 1 , nickel claim 1 , copper claim 1 , metal oxides thereof claim 1 , metal hydroxides thereof and metal-supported catalysts obtained by precipitating any one of them on a carrier selected from activated carbon claim 1 , alumina claim 1 , titania and silica.31. The production process according to claim 1 , wherein the basic compound is triethylamine.5. The production process according to claim 4 , wherein methyl ethyl ketone is used as a reaction solvent. The present invention relates to a process for producing an amine compound or a thiourea compound which is useful as an intermediate for a cyclic carbodiimide compound.Since the hydrolysis of a compound having an ester bond such as a polyester is promoted by a polar group such as a carboxyl group, it is proposed to reduce the concentration of the carboxyl group by using a sealing agent for a carboxyl group (Paten Document 1, Patent Document 2). A carbodiimide compound is used as the sealing agent for a carboxyl group.However, since this carbodiimide compound is a linear compound, a volatile isocyanate compound is by-produced during use and generates a bad odor, thereby deteriorating work environment.Then, the inventors of the present invention found as the sealing agent a cyclic carbodiimide compound which does not by-produce an isocyanate compound when it reacts with a carboxyl group and filed an international application (Patent Document 3). However, industrial processes for producing this useful cyclic carbodiimide compound and an intermediate therefor have not been established.It is an object of the present invention to improve the reaction yield of an amine compound represented by the following formula (B) when it is synthesized by ...

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Номер записи: 6

18-04-2013 дата публикации

Process for Preparation of Optically Active Compounds using Transfer Hydrogenation

Номер: US20130096337A1

Автор: Foulkes Michael, Kesselgruber Martin, Mathes Christian

Принадлежит: NOVARTIS AG

A catalytic process for the preparation of optically active compounds and their conversion thereafter to desired drug substances. In particular, the process relates to the preparation of (S)-3-(1-Dimethylamino-ethyl)-phenol using asymmetric catalytic reduction and transfer hydrogenation, thereby providing an improved route to forming drug substances such as rivastigimine and rivastigimine hydrogen tartrate. 139-. (canceled)42. The process of claim 41 , wherein the asymmetric catalytic reduction forms an enantiomeric excess of compound (III) to compound (IV) of from about 96%:4% or higher claim 41 , about 98%:2% or higher claim 41 , or about 99%:1% or higher.43. The process of claim 41 , wherein after a crystallization step the enantiomeric excess of compound (III) to compound (IV) is from about 97%:3% or higher claim 41 , about 98%:2% or higher claim 41 , about 99%:1% or higher claim 41 , or about >99.5%:about <0.5% claim 41 , or about >99.7%:about <0.03.%.44. The process of claim 41 , wherein n=1 in general formulas (I)-(IV).45. The process of claim 41 , wherein n=1 in general formulas (I)-(IV) and a hydroxyl group occurs at position 3 on the aromatic ring.46. The process of claim 40 , wherein Ris a Calkyl claim 40 , Calkenyl claim 40 , Calkynyl claim 40 , or Corganohalide.47. The process of claim 40 , wherein Ris selected from any of methyl claim 40 , ethyl claim 40 , propyl and butyl.49. The process of claim 40 , wherein the transfer hydrogenation is performed using a chiral transition metal based catalyst.50. The process of claim 40 , wherein the transfer hydrogenation is performed using a complexed transition metal based chiral catalyst containing multiple aryl claim 40 , mono- bi- claim 40 , or poly-dentate ligands.51. The process of claim 40 , wherein the transfer hydrogenation is performed using a Ru claim 40 , Rh or Ir based catalyst.52. The process of claim 40 , wherein the transfer hydrogenation is performed using a chiral (diphenylethylenediamine) based ...

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Номер записи: 7

18-04-2013 дата публикации

RESOLUTION METHODS FOR ISOLATING DESIRED ENANTIOMERS OF TAPENTADOL INTERMEDIATES AND USE THEREOF FOR THE PREPARATION OF TAPENTADOL

Номер: US20130096346A1

Автор: BONDGE Sandipan Prabhurao, Khunt Mayur Devjibhai, Pradhan Nitin Sharadchandra

Принадлежит: ACTAVIS GROUP PTC EHF

Provided herein is an improved and industrially advantageous optical resolution method for resolving (2R,3R)/(2S,3S)-1-dimethylamino-3-(3-methoxyphenyl)-2-methylpentan-3-ol, and use thereof for the preparation of tapentadol or a pharmaceutically acceptable salt thereof. Provided further herein is an improved and industrially advantageous optical resolution method for resolving (2R,3R)/(2S,3S)-[3-(3-methoxyphenyl)-2-methylpentyl]-dimethylamine, and use thereof for the preparation of tapentadol or a pharmaceutically acceptable salt thereof. Disclosed also herein is an improved, commercially viable and industrially advantageous process for the preparation of tapentadol or a pharmaceutically acceptable salt thereof in high yield and purity. 2. The process of claim 1 , wherein the first solvent used in step-(a) is selected from the group consisting of water claim 1 , an alcohol claim 1 , a ketone claim 1 , a cyclic ether claim 1 , an aliphatic ether claim 1 , a hydrocarbon claim 1 , a chlorinated hydrocarbon claim 1 , a nitrile claim 1 , an ester claim 1 , a polar aprotic solvent claim 1 , and mixtures thereof; wherein the second solvent used in step-(c) is selected from the group consisting of water claim 1 , an alcohol claim 1 , a ketone claim 1 , a cyclic ether claim 1 , an aliphatic ether claim 1 , a hydrocarbon claim 1 , a chlorinated hydrocarbon claim 1 , a nitrile claim 1 , an ester claim 1 , and mixtures thereof; and wherein the base used in step-(c) is selected from the group consisting of triethylamine claim 1 , trimethylamine claim 1 , dimethyl amine claim 1 , tert-butyl amine claim 1 , aqueous ammonia claim 1 , sodium hydroxide claim 1 , calcium hydroxide claim 1 , magnesium hydroxide claim 1 , potassium hydroxide claim 1 , lithium hydroxide claim 1 , sodium carbonate claim 1 , potassium carbonate claim 1 , sodium bicarbonate claim 1 , potassium bicarbonate claim 1 , lithium carbonate claim 1 , sodium tert-butoxide claim 1 , sodium isopropoxide and potassium ...

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Номер записи: 8

18-04-2013 дата публикации

NOVEL PROCESS FOR PREPARING HIGHLY PURE TAPENTADOL OR A PHARMACEUTICALLY ACCEPTABLE SALT THEREOF

Номер: US20130096347A1

Автор: BONDGE Sandipan Prabhurao, Khunt Mayur Devjibhai, Pagire Haushabhau Shivaji, Patil Nilesh Sudhir, Pradhan Nitin Sharadchandra

Принадлежит: ACTAVIS GROUP PTC EHF

Provided herein is a novel, commercially viable and industrially advantageous process for the preparation of 3-[(1R,2R)-3-(dimethylamino)-1-ethyl-2-methylpropyl]phenol (Tapentadol), or a pharmaceutically acceptable salt thereof, and its intermediates, in high yield and purity. Provided also herein are novel solid state forms of tapentadol intermediates and processes for their preparation thereof. Provided further herein is a purification process for preparing highly pure tapentadol hydrochloride. 2. The process of claim 1 , wherein the first solvent used in step-(a) is selected from the group consisting of water claim 1 , an alcohol claim 1 , an ether claim 1 , a hydrocarbon claim 1 , a chlorinated hydrocarbon claim 1 , a nitrile solvent claim 1 , a polar aprotic solvent claim 1 , and mixtures thereof; wherein the second solvent used in step-(b) is selected from the group consisting of a ketone claim 1 , a cyclic ether claim 1 , an aliphatic ether claim 1 , and mixtures thereof; wherein the third solvent used in step-(c) is selected from the group consisting of water claim 1 , an alcohol claim 1 , a ketone claim 1 , an ester claim 1 , a hydrocarbon claim 1 , a chlorinated hydrocarbon claim 1 , a polar aprotic solvent claim 1 , and mixtures thereof; wherein the fourth solvent used in step-(e) is selected from the group consisting of water claim 1 , an alcohol claim 1 , a ketone claim 1 , a cyclic ether claim 1 , an aliphatic ether claim 1 , a hydrocarbon claim 1 , a chlorinated hydrocarbon claim 1 , a nitrile claim 1 , an ester claim 1 , and mixtures thereof; and wherein the fifth solvent used in step-(f) is selected from the group consisting of water claim 1 , an alcohol claim 1 , a ketone claim 1 , a cyclic ether claim 1 , an aliphatic ether claim 1 , a hydrocarbon claim 1 , a chlorinated hydrocarbon claim 1 , a nitrile solvent claim 1 , and mixtures thereof3. The process of claim 2 , wherein the first solvent used in step-(a) is selected from the group consisting ...

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Номер записи: 9

16-05-2013 дата публикации

Adhesive Compositions for Bonding Composites

Номер: US20130123513A1

Автор: Rammon Richard M., Williamson Bobby Lee

Принадлежит: GEORGIA-PACIFIC CHEMICALS LLC

The present invention relates to a non-thermosetting composition made by reacting epichlorohydrin and a primary amine, to the use of that composition for making thermosetting (curable) adhesives suitable for bonding composites, to a method of preparing composites using the thermosetting (curable) adhesives, and to the related composites bonded with the thermosetting (curable) adhesives. 1. A non-thermosetting, reaction product of (a) epichlorohydrin and (b) an amine selected from the group consisting of ammonia, a primary amine and mixtures thereof, wherein the reaction product is produced by reacting the epichlorohydrin and the amine in a ratio of 0.40 to 0.92 moles of epichlorohydrin per atom equivalent of amine hydrogen and wherein the epi-amine reaction product is produced by reacting in a serial fashion separate portions of the epichlorohydrin and separate portions of the amine at a temperature of not greater than 60° C. This application is a divisional of co-pending U.S. patent application Ser. No. 12/718,391, filed on Mar. 5, 2010, which claims the benefit of U.S. Provisional Application No. 61/158,013 filed Mar. 6, 2009, each of which is hereby incorporated by reference in its entirety.The present invention is directed to a non-thermosetting composition made by reacting epichlorohydrin and an amine, to the use of that composition for making thermosetting (curable) adhesives, particularly adhesives suitable for bonding composites, to a method of preparing composites, particularly wood composites using the thermosetting (curable) adhesives, and to the related composites bonded with the cured thermosetting (curable) adhesives.A variety of composite materials are made by bonding into a unitary product a primary constituent, often a structural or reinforcement component, using a bonding agent or matrix material, such as an adhesive resin. Composites include engineered wood products (wood-adhesive composite products), insulation products and the like.Wood-adhesive ...

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Номер записи: 10

16-05-2013 дата публикации

LIQUID PHENOL RESIN AND METHOD OF PREPARING THE SAME

Номер: US20130123538A1

Автор: Suzuki Yuji

Принадлежит: SUMITOMO BAKELITE CO., LTD.

According to the present invention, a liquid phenol resin that has excellent characteristics of a phenol resin, such as thermal resistance and hardenability, and can produce a molded product having excellent flexibility, and a method of preparing the resin are provided. 1. A liquid phenol resin obtained by reacting (A) oils and (B) phenols with (C) a secondary and/or a tertiary alkylamine compound.2. The liquid phenol resin according to claim 1 , wherein the (A) oils include at least one or more kinds selected from the group consisting of cashew oil claim 1 , linseed oil claim 1 , tung oil claim 1 , castor oil claim 1 , and tall oil.3. The liquid phenol resin according to claim 1 , wherein a nitrogen content based on the whole liquid phenol resin is 3% by weight to 30% by weight.4. The liquid phenol resin according to claims 1 , wherein a weight ratio between the (A) oils and the (B) phenols is (A):(B)=10:90 to 90:10.5. The liquid phenol resin according to claim 1 , wherein the (C) secondary and/or tertiary alkylamine compound includes hexamethylenetetramine.6. The liquid phenol resin according to claim 1 , which is obtained by reacting the (A) oils and the (B) phenols with the (C) secondary and/or a tertiary alkylamine compound claim 1 , in a molar ratio of (C)/{(A)+(B)}=0.13 to 0.35.7. The liquid phenol resin according to claim 1 , which is used for impregnation.8. A method of preparing a liquid phenol resin which is the liquid phenol resin according to claim 1 , comprising reacting (A) oils and (B) phenols with (C) a secondary and/or a tertiary alkylamine compound without performing a step of dehydration. The present invention relates to a liquid phenol resin and a method of preparing the same.Priority is claimed on Japanese Patent Application No. 2010-167934, filed Jul. 27, 2010, the content of which is incorporated herein by reference.A phenol resin as a thermosetting resin is widely used mainly as a binder for binding materials that become a substrate of a ...

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Номер записи: 11

16-05-2013 дата публикации

Methods for preparing ritodrine hydrochloride

Номер: US20130123539A1

Автор: Jacopo Zanon

Принадлежит: Lundbeck Pharmaceuticals Italy SpA

Methods for preparing Ritodrine hydrochloride are provided. Also provided is non-hygroscopic, crystalline, polymorphic Ritodrine hydrochloride of Form I.

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Номер записи: 12

23-05-2013 дата публикации

Process for Producing SN-Comprising Catalysts

Номер: US20130131339A1

Автор: Baas Heiko, Heidemann Thomas, Kubanek Petr, Tsou Joana Coelho

Принадлежит: BASF SE

The present invention relates to a process for producing a supported tin-comprising catalyst, wherein a solution (S) comprising tin nitrate and at least one complexing agent is applied to the support, where the solution (S) does not comprise any solid or has a solids content of not more than 0.5% by weight based on the total amount of dissolved components. 120.-. (canceled)21. A process for producing a supported tin-comprising catalyst , wherein a solution (S) comprising tin nitrate and at least one complexing agent is applied to the support , where the solution (S) does not comprise any solid or comprises a solids content of not more than 0.5% by weight based on the total amount of dissolved components.22. The process according to claim 21 , wherein the solution (S) is an aqueous solution.23. The process according to claim 21 , wherein the solution (S) additionally comprises at least one further metal salt.24. The process according to claim 23 , wherein the further metal salt is nickel nitrate claim 23 , cobalt nitrate or copper nitrate.25. The process according to claim 21 , wherein the support is aluminum oxide.26. The process according to claim 21 , wherein the complexing agent is selected from among glycolic acid claim 21 , lactic acid claim 21 , hydracylic acid claim 21 , hydroxybutyric acid claim 21 , hydroxyvaleric acid claim 21 , malic acid claim 21 , mandelic acid claim 21 , citric acid claim 21 , sugar acids claim 21 , tartronic acid claim 21 , tartaric acid claim 21 , oxalic acid claim 21 , malonic acid claim 21 , maleic acid claim 21 , succinic acid claim 21 , glutaric acid claim 21 , adipic acid claim 21 , glycine claim 21 , hippuric acid claim 21 , EDTA claim 21 , alanine claim 21 , valine claim 21 , leucine and isoleucine.27. The process according to claim 21 , wherein the solution (S) comprises tin nitrate claim 21 , nickel nitrate claim 21 , cobalt nitrate claim 21 , copper nitrate and citric acid.28. The process according to claim 21 , wherein the ...

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Номер записи: 13

23-05-2013 дата публикации

BRANCHED SECONDARY ALCOHOL ALKOXYLATE SURFACTANTS FOR TEXTILE PROCESSING

Номер: US20130131386A1

Автор: Maynard Shawn J., Wang Xiao Hua, Yu Wanglin

Принадлежит: Dow Global Technologies LLC

Provided is a composition that is useful for textile processing, including for softening and providing smoothness to textiles The composition comprises an alkoxylate of the formula (I): wherein AO, EO, m, n, R. Rand Rare as defined below, and a polysiloxane oil 2. A composition according to wherein the polydispersity index of the alkoxylate is 1.15 or less.32. A composition according to any one of - wherein the composition comprises no more than 2 percent by weight of residual alcohol.43. A composition according to any one of - wherein AO is propyleneoxy or butyleneoxy.54. A composition according to any one of - wherein the group formed by R claims 1 , R claims 1 , Rand the carbon to which they are attached contains 9 to 12 carbon atoms.76. A composition according to any one of - wherein the polysiloxane oil is aminofunctionalized silicone oil claims 1 , amidofunctional silicone claims 1 , dimethylsilicone oil claims 1 , or hydroxyfunctional silicone.87. A composition according to any one of - where the composition is in the form of a concentrate.97. A composition according to any one of - where the composition further comprises water and is the form of an emulsion.10. A composition according to comprising 5 to 100 parts by weight of the alkoxylate and 20 to 2000 parts by weight of water claim 9 , based on 100 parts by weight of the polysiloxane oil.1110. A method for treating and processing textile materials which comprises contacting the textile materials with a composition according to any one of -.12. A textile treated by the method of . The invention relates to new branched secondary alcohol alkoxylates, to compositions thereof, and to their use in textile processing.Polysiloxanes are used in the textile processing industry as finishing agents for improving various properties of the textile, such as smoothness and softness. Typically, the polysiloxanes are employed in the form of oil-in-water emulsions, prepared by emulsification of a polysiloxane using a ...

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Номер записи: 14

13-06-2013 дата публикации

STEREOSELECTIVE SYNTHESIS OF TAPENTADOL AND ITS SALTS

Номер: US20130150622A1

Автор: Fandrick Daniel Robert, RODRIGUEZ Sonia, YANG Bing-Shiou

Принадлежит: BOEHRINGER INGELHEIM INTERNATIONAL GMBH

A process for the synthesis of a salt of tapentadol. 2. The process according to claim 1 , wherein the suitable solvent of steps (a) to (g) are each organic solvents claim 1 , preferably anhydrous organic solvents.3. The process according to claim 1 , wherein the suitable solvent of step (a) is anhydrous dimethylformamide (DMF) claim 1 , anhydrous dimethylsulfoxide (DMSO) claim 1 , anhydrous dimethyl acetamide (DMAc) claim 1 , anhydrous ethanol claim 1 , anhydrous methanol claim 1 , anhydrous n-propanol claim 1 , anhydrous 2-butanol claim 1 , anhydrous 1-butanol claim 1 , anhydrous tetrahydrofuran (THF) claim 1 , anhydrous 2-methyltetrahydrofuran (2-MeTHF) claim 1 , anhydrous dioxane claim 1 , anhydrous toluene claim 1 , anhydrous ethyl acetate claim 1 , anhydrous isopropyl acetate claim 1 , or a mixture thereof.4. The process according to claim 1 , wherein the suitable solvent of step (b) is anhydrous 2-MeTHF claim 1 , anhydrous THF claim 1 , anhydrous toluene claim 1 , anhydrous dioxane claim 1 , anhydrous methyl tert-buyl ether (MTBE) claim 1 , anhydrous cyclopentyl methyl ether claim 1 , or anhydrous diethyl ether.5. The process according to claim 1 , wherein step (b) is accomplished using a suitable reducing agent claim 1 , the reducing agent preferably selected from lithium borohydride claim 1 , sodium borohydride claim 1 , lithium aluminum hydride claim 1 , disobutyl aluminum hydride claim 1 , or RedAl.6. The process according to claim 1 , wherein the suitable solvent of step (c) is THF claim 1 , 2-MeTHF claim 1 , toluene claim 1 , dioxane claim 1 , MTBE claim 1 , cyclopentyl methyl ether claim 1 , diethyl ether claim 1 , or a mixture thereof.7. The process according to claim 1 , wherein claim 1 , the organometallic catalyst of step (d) is [Ir(COD)Cl]or [Ir(COE)Cl].8. The process according to claim 1 , wherein the suitable solvent of step (d) is dichloromethane claim 1 , THF claim 1 , toluene claim 1 , dioxane claim 1 , MTBE claim 1 , cyclopentyl methyl ether ...

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Номер записи: 15

27-06-2013 дата публикации

PROCESS FOR THE DIRECT AMINATION OF SECONDARY ALCOHOLS WITH AMMONIA TO GIVE PRIMARY AMINES

Номер: US20130165672A1

Автор: Deutsch Jens, Haas Thomas, Klasovsky Florian, Koeckritz Angela, Martin Andreas, Pfeffer Jan Christoph, Tacke Thomas

Принадлежит: EVONIK DEGUSSA GmbH

The invention relates to a process for preparing primary amines which comprises the process steps 1. A process for preparing a primary amine , the process comprising:i) providing a solution of a secondary alcohol in a fluid, nongaseous phase, free ammonia, at least one ammonia-releasing compound, or both,', 'and a homogeneous catalyst, and, 'ii) contacting the solution with'} 'wherein:', 'iii) optionally isolating the primary amine obtained in said contacting ii),'}a) a volume ratio of a liquid phase to a gas phase in said contacting ii) is greater than or equal to 0.25, orb) a molar ratio of the ammonia to hydroxyl groups in the secondary alcohol is at least 5:1, orboth a) and b).2. The process according to claim 1 , wherein the homogeneous catalyst isan alkali metal alkoxide, an aluminium alkoxide, a lanthanide alkoxide, an inorganic compound of noble metals,a monometallic or multimetallic, mononuclear or multinuclear coordination compound of at least one noble metal selected from the group consisting of ruthenium, iridium, rhodium, osmium, palladium, platinum and iron,or any mixture thereof.3. The process according to claim 1 ,whereinthe secondary alcohol comprises at least two secondary hydroxy groups.4. The process according to claim 1 ,whereinthe secondary alcohol comprises a cyclic or polycyclic carbon skeleton.5. The process according to claim 1 ,whereinthe secondary alcohol is selected from the group consisting of:2-dodecanol, cyclododecanol, 4-phenyl-2-butanol, isosorbide, isomannide, isoidite, polypropylene glycol, mannitol, sorbitol, galactitol and an alkyl glycoside.6. The process according to claim 1 ,whereinthe secondary alcohol is selected from the group consisting of an alpha-hydroxycarboxylic acid and an OH-modified, natural fatty acid.7. The process according to claim 1 ,wherein a liquid or supercritical ammonia, a solution of ammonium salts in a solvent, or both is used in said contacting ii).8. The process according to claim 1 ,whereinsaid ...

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Номер записи: 16

27-06-2013 дата публикации

PROCESS FOR THE SYNTHESIS OF CHOLINE SALTS

Номер: US20130165694A1

Автор: Lustig Steven Raymond, Redder Dennis A.

Принадлежит: E I DU PONT DE NEMOURS AND COMPANY

A method to synthesize choline salts to be used as inexpensive ingredients for application in ionic liquids or other applications is disclosed. 1. A process for the synthesis of one or more choline salts , comprising:(a) providing an aqueous solution of choline;(b) combining the aqueous solution of choline with a hydrophobic organic solvent and an excess of free acid to form a first acidic, solution;(c) combining the first acidic solution with one or more alcohols to form a first extraction mixture;(d) separating the first extraction mixture into a lower phase, a middle phase and an upper phase; and(e) recovering the lower phase of the first extraction mixture to provide a first aqueous solution of a choline salt.2. A process according to further comprising:(f) combining the first aqueous solution of choline salt with an excess of free acid and a hydrophobic organic solvent to form a second acidic solution;(g) combining the second acidic solution with at least one alcohol and to form a second extraction mixture;(h) separating the second extraction mixture into a lower phase, a middle phase and an upper phase; and(i) recovering the lower phase of the second extraction mixture to provide a second aqueous solution of a choline salt.3. A process according to further comprising isolating the choline salt from the first aqueous solution of choline salt.4. A process according to further comprising isolating the choline salt from the second. aqueous solution of choline salt.5. A process according to further comprising recycling the hydrophobic organic solvent for further use in the process.4. A process according to wherein the alcohol comprises at least one Cto Calcohol.5. A process according to wherein the alcohol comprises ethanol claim 1 , propanol or isopropanol.6. A process according to wherein the hydrophobic organic solvent comprises a high-boiling-point alkane.7. A process according to wherein the hydrophobic organic solvent comprises cyclohexane.8. A process ...

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Номер записи: 17

04-07-2013 дата публикации

METHOD FOR PRODUCTION OF F-18 LABELED AMYLOID BETA LIGANDS

Номер: US20130172620A1

Автор: Berndt Mathias, FRIEBE Matthias, Hultsch Christina, PATT Marianne, Samson Fabrice, Schildan Andreas, Smuda Christoph

Принадлежит: PIRAMAL IMAGING SA

This invention relates to methods, which provide access to [F-18]fluoropegylated (aryl/heteroaryl vinyl)-phenyl methyl amine derivatives. 2. A method according to claim 1 , wherein PG is selected from the group consisting of:a) Boc,b) Trityl andc) 4-Methoxytrityl.3. A method according to claim 1 , wherein LG is selected from the group consisting of:a) Halogen andb) Sulfonyloxy,Wherein Halogen is chloro, bromo or iodo.4. A method according to claim 3 , wherein Sulfonyloxy is selected from the group consisting of:a) Methanesulfonyloxy,b) p-Toluenesulfonyloxy,c) (4-Nitrophenyl)sulfonyloxy,d) (4-Bromophenyl)sulfonyloxy.5. A method according to claim 1 , wherein n=3 and X═CH.6. A method according to claim 1 , wherein n=3 claim 1 , X═CH claim 1 , R=Boc claim 1 , and LG=Methanesulfonyloxy.7. A method according to claim 1 , wherein the radiofluorination reaction is carried out in a mixture of acetonitrile and co-solvents claim 1 , wherein the percentage of acetonitrile is at least 50%.8. A method according to claim 7 , wherein the radiofluorination reaction is carried out in a mixture of acetonitrile and co-solvents claim 7 , wherein the percentage of acetonitrile is at least 70%.9. A method according to claim 7 , wherein the radiofluorination reaction is carried out in a mixture of acetonitrile and co-solvents claim 7 , wherein the percentage of acetonitrile is at least 90%.10. A method according to claim 1 , wherein 1.5-75 μmol claim 1 , preferably 10-30 μmol and even more preferably 12-25 μmol of compound of Formula II are used in Step 1.11. A method according to claim 1 , wherein the method is performed as a fully automated process.12. A kit claim 1 , comprising a sealed vial comprising a predetermined quantity of a compound of formula II of and a sealed vial comprising acetonitrile or acetonitrile and a co-solvent.13. A method according to claim 1 , wherein Step 3 comprises a purification by HPLC.14. A method according to claim 13 , wherein the HPLC solvent used in ...

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Номер записи: 18

04-07-2013 дата публикации

INTEGRATED PROCESSES FOR THE PREPARATION OF POLYBENZIMIDAZOLE PRECURSORS

Номер: US20130172621A1

Автор: Dhawan Rajiv, Hargis Annalisa, Ritter Joachim C.

Принадлежит: E.I.DU PONT DE NEMOURS AND COMPANY

An integrated process is provided for efficiently preparing 2,4,5-triaminophenol, starting with nitration of 2,6-dihalobenzene; high purity salts thereof; and complexes of 2,4,5-triaminophenol aromatic diacids, which are precursors for making polybenzimidazole polymer for high performance fibers. The process design eliminates several costly intermediate drying and recrystallization steps. The handling of solid materials with possible skin sensitizing properties and toxicity is avoided, thereby eliminating human and environmental exposure. 2. The process of further comprising slurrying or dissolving the 2 claim 1 ,4 claim 1 ,5-triaminophenol product in water; adding an acid to the slurry to form and precipitate 2 claim 1 ,4 claim 1 ,5-triaminophenol salt; and cooling claim 1 , filtering claim 1 , and washing the precipitated 2 claim 1 ,4 claim 1 ,5-triaminophenol salt.3. The process of wherein the acid in step (j) is selected from the group consisting of HCl claim 1 , acetic acid claim 1 , HSO claim 1 , and HPO.4. The process of wherein Z═Cl and the acid in step (j) is HCl.5. The process of wherein the solvent used in step (e) is distilled and recycled.6. The process of wherein the spent hydrogenation catalyst of step (k) is recovered and recycled.7. The process of wherein the acid added to the slurry to form and precipitate 2 claim 2 ,4 claim 2 ,5-triaminophenol salt is selected from the group consisting of HCl claim 2 , acetic acid claim 2 , HSO claim 2 , and HPO.8. The process of wherein the precipitated salt is washed with water and methanol claim 2 , and the methanol is recycled.9. The process of further comprising drying the 2 claim 2 ,4 claim 2 ,5-triaminophenol salt.10. The process of further comprising adding a reducing agent to at least one aqueous suspension or aqueous solution containing 2 claim 1 ,4 claim 1 ,5-triaminophenol or 2 claim 1 ,4 claim 1 ,5-triaminophenol salt.11. The process of claim 10 , wherein the reducing agent is tin powder.12. The ...

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Номер записи: 19

04-07-2013 дата публикации

PROCESS FOR MAKING TERTIARY AMINOALCOHOL COMPOUNDS

Номер: US20130172622A1

Автор: Moore David W., Peera Asghar A., Swedo Raymond J.

Принадлежит: ANGUS Chemical Company

Provided is a process for making a tertiary aminoalcohol compound. The process comprises using an excess amount of a carbonyl compound in a condensation step between the carbonyl compound and a nitroalkane, and conducting a hydrogenation/alkylation step to produce the tertiary aminoalcohol. The process uses fewer steps than conventional processes. 2. The process of wherein the intermediate product mixture of step (a) comprises at least two moles of free carbonyl compound of formula III per mole of nitroalcohol compound of formula II.3. The process of wherein additional carbonyl compound of formula III is added following step (b).4. The process of wherein Rand Rare each independently C-Calkyl.5. The process of wherein Rand Rare each —C(OH)RR.6. The process of wherein Ris —C(OH)RRand Ris C-Calkyl.7. The process of wherein Rand Rtogether with the carbon to which they are attached form C-Ccycloalkyl.8. The process of wherein Rand Rare H.9. The process of wherein following step (b) claim 1 , the concentration of the tertiary aminoalcohol compound of formula I in the intermediate product mixture is at least 0.5 percent by weight.10. The process of wherein the compound of formula I is 2-(dimethylamino)-2-methyl-1-propanol claim 1 , N claim 1 ,N-dimethyltris(hydroxymethyl)aminomethane claim 1 , 2-(dimethylamino)-2-ethylpropane-1 claim 1 ,3-diol claim 1 , 2-(dimethylamino)-2-methylpropane-1 claim 1 ,3-diol or 1-(dimethylamino)cyclohexylmethanol. The invention relates to an improved process for making tertiary aminoalcohol compounds.Tertiary aminoalcohol compounds play an important role in a variety of commercial and consumer products. For instance, they may be used as neutralizers in paints and coatings, in process water applications, and personal care and cosmetics formulations, as emulsifying agents, as corrosion inhibitors, e.g., in metalworking fluids, as resin solubilizers, foam catalysts, finish stabilizers, and/or as raw materials for chemical synthesis of other ...

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Номер записи: 20

25-07-2013 дата публикации

PROCESS FOR PREPARING L-PHENYL-3-DIMETHYLAMINOPROPANE DERIVATIVE

Номер: US20130190522A1

Автор: BHIRUD Shekhar Bhaskar, Jamshad Danish, Johar Perminder Singh, Mishra Sushanta

Принадлежит: IND-SWIFT LABORATORIES LIMITED

Provided is a process for the preparing 1-phenyl-3-dimethylaminopropane derivatives of formula I, (The formula should be inserted here) and its pharmaceutically acceptable salts thereof via novel intermediates. 2. (canceled)3. The process according to claim 28 , wherein in step a) claim 28 , the suitable reagent is an optionally substituted sulfonyl halide or an optionally substituted sulfonyl anhydride;said sulfonyl halide being selected from the group consisting of a linear or branched alkylsulfonyl halide, an arylsulfonyl halide, an aralkylsulfonyl halide, an alkarylsulfonyl halide, a heteroalkylsulfonyl halide, a heteroarylsulfonyl halide, p-toluenesulfonyl halide, benzenesulfonyl halide, ortho-chlorobenzenesulfonyl halide, meta-chlorobenzenesulfonyl halide and para-chlorobenzenesulfonyl halide; andsaid sulfonyl anhydride being selected from the group consisting of a linear or branched alkylsulfonyl anhydride, an arylsulfonyl anhydride, an aralkylsulfonyl anhydride, an alkarylsulfonyl anhydride, a heteroalkylsulfonyl anhydride, or a heteroarylsulfonyl anhydride.4. The process according to claim 28 , wherein in step b) claim 28 , the suitable aminomethyling agent is formaldehyde and dimethyl amine; or N-methyl-N-methylenemethane ammonium halide and acetyl halide.5. (canceled)6. (canceled)7. (canceled)8. The process according to claim 1 , wherein in step b) claim 1 , the suitable organometallic reagent is ethyl lithium or an ethyl magnesium halide.9. The process according to claim 1 , wherein in step c) the suitable acid is selected from the group consisting of:the inorganic acids hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, and perchloric acid;the achiral organic acids formic acid and acetic acid; andthe chiral organic acids camphor sulfonic acid, mandelic acid, and substituted or unsubstituted tartaric acid; andmixtures thereof.10. The process according to claim 1 , wherein in step d) claim 1 , the suitable dehydrating agent is selected from ...

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Номер записи: 21

25-07-2013 дата публикации

PROCESS FOR PREPARING CHOLINE HYDROXIDE FROM TRIMETHYLAMINE AND ETHYLENE OXIDE

Номер: US20130190534A1

Автор: Chen Xiaoyun, Dixit Ravindra S., JR. John G., Li Ruokang, Patel Avani M., Pell Randy J., PENDERGAST

Принадлежит: DOW AGROSCIENCES LLC

Processes for preparing N,N,N-trimethylethanolammonium hydroxide (choline hydroxide) and the choline hydroxide produced are described. These processes minimize the production of byproduct mono-ethoxylated and di-ethyoxylated choline in the product choline hydroxide. The processes generally include feeding ethylene oxide, trimethylamine, and water into a first reactor to create a first reactor product under temperature controlled conditions. The product of the first reactor is fed into a second reactor to form a second reactor product under uncontrolled, adiabatic, conditions. Finally, any unreacted to trimethylamine in the second reactor product is removed to form a final product comprising choline hydroxide. Additional reactors can be used for the ethylene oxide and trimethylamine reaction. 1. A process for preparing choline hydroxide comprising:feeding ethylene oxide, trimethylamine, and water into a first reactor to create a first reactor product, wherein the first reactor temperature is maintained between 5° C. and 35° C. and the molar ratio of ethylene oxide to trimethylamine fed to the first reactor is equal to or less than one;feeding the first reactor product into a second reactor to form a second reactor product, wherein the second reactor is insulated; andremoving any unreacted trimethylamine from the second reactor product to form a final product comprising choline hydroxide.2. The process of claim 1 , wherein the choline hydroxide final product comprises less than 10 weight percent mono-ethoxylated choline and/or di-ethyoxylated choline.32. The process of any one of - claims 1 , wherein the trimethylamine and water are fed into the first reactor as a mixture.43. The process of any one of - claims 1 , wherein the residence time in the second reactor is sufficient for any unreacted ethylene oxide present in the first reactor product to react.54. The process of any one of - claims 1 , wherein adiabatic heating in the second reactor raises the temperature of ...

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Номер записи: 22

01-08-2013 дата публикации

Short synthesis of tolterodine, intermediates and metabolites

Номер: US20130197082A1

Автор: Damjan Sterk

Принадлежит: Lek Pharmaceuticals dd

A process is described for the preparation of intermediates which can be used for preparation of agents for urinary incontinence therapy, specifically to 2-(3-(diisopropylamino)-1-phenylpropyl)-4-(hydroxymethyl)phenol and its prodrugs.

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Номер записи: 23

01-08-2013 дата публикации

PROCESSES FOR THE PREPARATION OF FESOTERODINE

Номер: US20130197260A1

Автор: DWIVEDI Shriprakash Dhar, JAIN Kuldeep Natwarlal, PRASAD Ashok

Принадлежит: CADILA HEALTHCARE LIMITED

The invention relates to improved process for the preparation of fesoterodine and its pharmaceutically acceptable salt, specifically fesoterodine fumarate of formula (1). The invention relates to solid state forms of a novel salt of fesoterodine and process for the preparation thereof. The invention also relates to highly pure fesoterodine fumarate substantially free of impurity X at RRT 1.37. The invention also provides solid particles of pure fesoterodine fumarate wherein 90 volume-percent of the particles (D90) have a size of higher than 200 microns. 1. Fesoterodine 2-chloro-mandelate.2. The fesoterodine 2-chloro-mandelate as claimed in claim 1 , which is in a crystalline form or an amorphous form.3. The fesoterodine 2-chloro-mandelate as claimed in claim 1 , wherein 2-chloro-mandelic acid is racemic(±) 2-chloro-mandelic acid claim 1 , S-(+)-2-chloro-mandelic acid claim 1 , or R-(−)-2-chloro-mandelic acid.4. The festerodine 2-chloro mandelate as claimed in claim 3 , wherein the 2-chloro-mandelic acid is S-(+)-2-chloro-mandelic acid.5. Fesoterodine 2-chloro-mandelate as claimed in claim 1 , with one or more of the following properties:i) a powder X-ray diffraction pattern having peaks at about 9.9, 12.9, 14.2, 19.2, 20.7 and 24.9±0.2 degrees 2-theta;{'figref': {'@idref': 'DRAWINGS', 'FIG. 5'}, 'ii) a powder X-ray diffraction pattern as depicted in ;'}{'figref': {'@idref': 'DRAWINGS', 'FIG. 6'}, 'iii) a DSC thermogram having an endotherm peak at about 162° C. or substantially as depicted in ; or'}{'sup': '−1', 'figref': {'@idref': 'DRAWINGS', 'FIG. 7'}, 'iv) an infrared spectrum having absorption bands at about 3346, 2985, 2970, 2939, 2873, 2603, 2368, 1755, 1620, 1492, 1388, 1328, 1224, 1190, 1120, 1087, 1062, 1031, 970, 916, 867, 819, 759, 732, 705, 607, 582. 561, 522 and 501 cmor a spectrum depicted in .'}6. A process for the preparation of fesoterodine 2-chloro-mandelate claim 1 , the process comprising obtaining a solution of fesoterodine in one or more ...

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Номер записи: 24

22-08-2013 дата публикации

INTERMEDIATE COMPOUNDS AND PROCESS FOR THE PREPARATION OF FINGOLIMOD

Номер: US20130217899A1

Автор: Marom Ehud, Mizhiritskii Michael, Rubnov Shai

Принадлежит: MAPI PHARMA LTD.

The present invention relates to processes for the preparation of (2-Amino-2-[2-(4-octylphenyl)ethyl]propane-1,3-diol hydrochloride (Fingolimod) and pharmaceutically acceptable salts thereof, and intermediates formed in such processes. 142-. (canceled)44. The process according to claim 43 , wherein step (a) is conducted in the presence of a Friedel-Crafts catalyst claim 43 , a metal salt of an organic acid claim 43 , or a protic acid claim 43 , wherein{'sub': 3', '3', '4', '4', '2', '3, 'the Friedel Crafts catalyst is selected from AlCl, FeCl, SnCl, TiCl, ZnCland BF;'}the metal salt of an organic acid is a metal triflate selected from hafnium triflate and cerium triflate; and{'sub': 2', '4', '3', '3, 'the protic acid is selected from HF, HSO, CFSOH and an ion-exchange resin which is selected from Nafion or zeolite.'}45. The process according to claim 43 , wherein the reducing agent in step (b) is NaBH.46. The process according to claim 43 , wherein the hydroxy protecting group P in compound (13A) is acetyl (COCH) claim 43 , and wherein in step (c) the protection of 3-nitro-1-(4-octylphenyl)propan-1-ol is carried out by acylation with acetic anhydride or acetyl chloride in the presence of a base.47. The process according to claim 43 , whereinthe reduction of 3-nitro-1-(4-octylphenyl)propan-1-one (12) to 3-nitro-1-(4-octylphenyl)propan-1-ol and its conversion to compound (13A) is carried out in one step without isolation of intermediates; orwherein in step (d) the bis-hydroxymethylation of compound (13A) is carried out with formaldehyde or paraformaldehyde in the presence of a base; orwherein in step (d) the bis-hydroxymethylation of compound (13A) and deprotection to compound (14) is carried out in one step without isolation of intermediates.48. The process according to claim 43 , wherein the reduction step (e) comprises hydrogenating compound (14) to Fingolimod (1) in the presence of a Pd/C catalyst.50. The process according to claim 49 , wherein step (a) is ...

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Номер записи: 25

22-08-2013 дата публикации

METHOD FOR PRODUCTION OF F-18 LABELED AMYLOID BETA LIGANDS

Номер: US20130217920A1

Автор: Berndt Mathias, FRIEBE Matthias, Hultsch Christina, Oh Seung Jun, Samson Fabrice, Smuda Christoph

Принадлежит: PIRAMAL IMAGING SA

This invention relates to methods, which provide access to [F-18]fluoropegylated (aryl/heteraryl vinyl)-phenyl methyl amine derivatives. 2. A method according to claim 1 , wherein PG is selected from the group consisting of:a) Boc,b) Trityl andc) 4-Methoxytrityl.3. A method according to claim 1 , wherein LG is selected from the group consisting of:a) Halogen andb) Sulfonyloxy,Halogen is chloro, bromo or iodo.4. A method according to claim 3 , wherein Sulfonyloxy is selected from the group comprising:a) Methanesulfonyloxy,b) p-Toluenesulfonyloxy,c) (4-Nitrophenyl)sulfonyloxy,d) (4-Bromophenyl)sulfonyloxy.5. A method according to claim 1 , wherein n=3 and X=CH.6. A method according to claim 1 , wherein n=3 claim 1 , X=CH claim 1 , R=Boc claim 1 , and LG=Methanesulfonyloxy.7. A method according to claim 1 , wherein 10-50 μmol of a compound of formula II is used.8. A method according to claim 7 , wherein 10-30 μmol of a compound of formula II is used.9. A method according to claim 1 , wherein 10 or more μmol of a compound of formula II is used.10. A method according to claim 1 , wherein the method is performed as a fully automated process. This invention relates to methods, which provide access to [F-18]fluoropegylated (aryl/heteraryl vinyl)-phenyl methyl amine derivatives.Alzheimer's Disease (AD) is a progressive neurodegenerative disorder marked by loss of memory, cognition, and behavioral stability. AD is defined pathologically by extracellular senile plaques comprised of fibrillar deposits of the beta-amyloid peptide (Aβ) and neurofibrillary tangles comprised of paired helical filaments of hyperphosphorylated tau. The 39-43 amino acids comprising Aβ peptides are derived from the larger amyloid precursor protein (APP). In the amyloidogenic pathway, Aβ peptides are cleaved from APP by the sequential proteolysis by beta- and gamma-secretases. Aβ peptides are released as soluble proteins and are detected at low level in the cerebrospinal fluid (CSF) in normal aging ...

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Номер записи: 26

29-08-2013 дата публикации

QUATERNIZED POLYETHER AMINES AND THEIR USE AS ADDITIVE FOR FUELS AND LUBRICANTS

Номер: US20130225463A1

Автор: BOEHNKE Harald, Grabarse Wolfgang, HANSCH Markus, VOELKEL Ludwig, WALTER Marc

Принадлежит:

The present invention relates to novel quaternized polyetheramines and to the preparation thereof. The present invention further relates to the use of these compounds as a fuel and lubricant additive. More particularly, the invention relates to the use of these quaternized nitrogen compounds as a fuel additive for reducing or preventing deposits in the injection systems of direct injection diesel engines, especially in common rail injection systems, for reducing the fuel consumption of direct injection diesel engines, especially of diesel engines with common rail injection systems, and for minimizing power loss in direct injection diesel engines, especially in diesel engines with common rail injection systems. The invention also provides additive packages comprising these polyetheramines; and fuels and lubricants additized therewith. The invention further relates to the use of these quaternized nitrogen compounds as an additive for gasoline fuels, especially for improving the intake system cleanliness of gasoline engines. 1. A fuel composition or lubricant composition comprising , in a conventional fuel or lubricant , at least one reaction product comprising a quaternized nitrogen compound , said reaction product being obtainable by reactiona) of a polyether-substituted amine comprising at least one tertiary quaternizable amino group withb) a quaternizing agent which converts the at least one tertiary amino group to a quaternary ammonium group.2. The fuel composition or lubricant composition according to claim 1 , in which the polyether substituent comprises monomer units of the general formula Ic{'br': None, 'sub': 3', '4, '—[—CH(R)—CH(R)—O—]—\u2003\u2003(Ic)'}in which{'sub': 3', '4, 'Rand Rare the same or different and are each H, alkyl, alkylaryl or aryl.'}3. The fuel composition or lubricant composition according to claim 2 , wherein the polyether-substituted amine has a number-average molecular weight in the range from 500 to 5000.4. The fuel composition or ...

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Номер записи: 27

29-08-2013 дата публикации

SALTS OF POTASSIUM ATP CHANNEL OPENERS AND USES THEREOF

Номер: US20130225806A1

Автор: Cowen Neil M., Yamout Khaled A.

Принадлежит: Essentialis, Inc.

Provided are immediate or prolonged administration of certain salts of Kchannel openers such as diazoxide to a subject to achieve novel pharmacodynamic, pharmacokinetic, therapeutic, physiological, metabolic and compositional outcomes in the treatment of diseases or conditions involving Kchannels. Also provided are pharmaceutical formulations, methods of administration and dosing of the salts that achieve these outcomes and reduce the incidence of adverse effects in treated individuals. Further provided are method of co-administering the salts with other drugs to treat diseases of humans and animals. 2. The method of wherein said cation source is an alkali metal hydroxide.3. The method of wherein said cation source is sodium hydroxide or potassium hydroxide.4. The method of wherein said solvent is selected from the group consisting of acetonitrile claim 3 , low molecular weight ketones claim 3 , and tetrahydrofuran.5. The method of wherein said cation source is an organic cation source comprising an ammonium or at least one tertiary amine group.6. The method of wherein said cation source is choline hydroxide or hexamethyl hexamethylene diammonium dihydroxide.7. The method of wherein said solvent is selected from the group consisting of acetonitrile claim 6 , low molecular weight ketones claim 6 , tetrahydrofuran claim 6 , and 2-methyl tetrahydrofuran.8. The method of wherein said cation source is choline hydroxide claim 6 , and said solvent is selected from the group consisting of acetonitrile claim 6 , low molecular weight ketones claim 6 , tetrahydrofuran claim 6 , and 2-methyl tetrahydrofuran.9. The method of wherein said compound of Formulae I-IV is dissolved in a solvent at a ratio of about 1 g compound of Formulae I-IV to about 1 to 5 mL solvent.10. The method of further comprising adding a co-solvent prior to the step of removing the solvent.11. The method of wherein said co-solvent is selected from the group consisting of methyl tert-butyl ether (MTBE) claim ...

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Номер записи: 28

24-10-2013 дата публикации

BENZYLAMINE HYDROPHOBE

Номер: US20130281617A1

Автор: Bobsein Barrett R., Rabasco John J.

Принадлежит:

The present invention relates to a compound characterized by the following formula: 3. The compound of wherein Ris n-butyl or 2-ethylhexyl.7. The method of wherein Ris n-butyl or 2-ethylhexyl; m is 0; and p is 1. The present invention idea relates to an amine-based hydrophobe useful in preparing hydrophobically modified alkylene oxide urethane polymers, which are useful as rheology modifiers for coatings formulations.Rheology modifiers are typically designed to impart desirable rheological properties to coating formulations over a wide shear rate range. U.S. Pat. No. 7,741,402 discloses ethylene oxide urethane polymers modified with hydrophobes that contain organic bases such as secondary or tertiary amines (amine-modified HEURs), the presence of which provides for viscosity control through a pH trigger. When the pH of the HEUR composition is sufficiently low with respect to the pKof the incorporated base, the basic groups are protonated and the viscosity is relatively low; when the pH is sufficiently high, associative thickening occurs. Thus, incorporation of basic hydrophobes into the HEUR polymer allows relatively high concentration of polymer to be dissolved in water at low pH; once the solution is added to the high pH environment of paint coatings, the base is deprotonated and the associative thickening mechanism activated.Amine-modified HEURs can be sensitive to the pH of the paint formulation to which it is added. For example, the pH of the formulation, through time and heat aging, may decrease to a level below a critical pH conducive to associative thickening, thereby resulting in a poorer formulation; consequently, it would be desirable to discover a hydrophobe, more particularly an amine-based hydrophobe, that preserves the desired viscosity of the formulation in face of pH-lowering mechanisms.The present invention addresses a need by providing, in one aspect, a compound characterized by the following formula:where Ris C-C-alkyl, phenyl, naphthyl, C-C- ...

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Номер записи: 29

07-11-2013 дата публикации

NOVEL STEREOSPECIFIC SYNTHESIS OF (-) (2S, 3S)-1-DIMETHYLAMINO-3-(3-METHOXYPHENYL)-2-METHYL PENTAN-3-OL

Номер: US20130296608A1

Автор: Haritha Kirla, Krishnareddy Pingili, Mohan Rao Dodda, Ramachandrareddy Pingili, SRINIVAS Kolluru

Принадлежит: SYMED LABS LIMITED

The present invention relates to a novel stereospecific synthesis of (−)(2S,3S)-1-dimethylamino-3-(3-methoxyphenyl)-2-methyl pentan-3-ol an intermediate in the synthesis of 3-[(1R,2R)-3-(dimethylamino)-1-ethyl-2-methylpropyl]phenol. 18-. (canceled)10. The process of wherein the solvent employed is selected from the group consisting of ethers claim 9 , halo carbonated solvents claim 9 , and esters.11. The process of wherein the ether is selected from the group consisting of tetrahydrofuran (THF) claim 10 , 1 claim 10 ,4-dioxane claim 10 , diethyl ether or mixtures thereof.12. The process of wherein the halo carbonated solvent is selected from the group consisting of methylene chloride claim 10 , ethylene dichloride claim 10 , chloroform claim 10 , chlorobenzene claim 10 , dichlorobenzene and mixtures thereof.13. The process of wherein the ester is selected from the group consisting of ethyl acetate claim 10 , isopropyl acetate claim 10 , n-butyl acetate claim 10 , tert-butyl acetate and mixtures thereof.14. The process of wherein the solvent is tetrahydrofuran.15. The process of wherein the reaction is performed at a temperature from about 0° C. to about 100° C.16. The process of wherein the reaction is performed at the boiling point of the solvent(s) used.17. The process of wherein the reaction is performed at about 25° C.18. The process of wherein the reaction is carried out at a time period from about 15 minutes to about 10 hours.19. The process of wherein the reaction is carried out at a time period from about 30 minutes to about 2 hours.20. The process of wherein the molar equivalent of the compound of formula IV and reagent used is from about 0.25 to about 7 molar equivalents on the weight of the compound of formula V.21. The process of wherein the molar equivalent of the compound of formula IV and reagent used is about 1 molar equivalent on the weight of the compound of formula V.22. The process of wherein the compound of the formula III obtained has a purity ...

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Номер записи: 30

14-11-2013 дата публикации

PRODUCTION METHOD FOR AMINO COMPOUND

Номер: US20130303805A1

Автор: Kuwahara Hisayuki, Wada Tomotaka

Принадлежит: MITSUBISHI GAS CHEMICAL COMPANY, INC.

The present invention relates to a process for producing an amino compound by subjecting a polyamine and an alkenyl compound to addition reaction in the presence of an alkali metal hydride compound which is capable of supplying the amino compound in a stable manner without occurrence of odor. 1: A process for producing an amino compound , the process comprising:conducting an addition reaction between a polyamine and an alkenyl compound in the presence of an alkali metal hydride compound.2: The process according to claim 1 ,wherein the conducting comprises mixing and contacting the alkali metal hydride compound with the polyamine, thereby obtaining a mixture and adding the alkenyl compound to the mixture.3: The process according to claim 1 ,wherein the conducting comprises adding the alkenyl compound intermittently in divided parts.4: The process according to claim 1 ,wherein the alkali metal hydride compound is present in an amount of from 0.01% to 3% by mass on a basis of a total amount of the alkali metal hydride compound and the polyamine.5: The process according to claim 1 , {'br': None, 'H2N—CH2-A-CH2—NH2\u2003\u2003(1),'}, 'wherein the polyamine is a polyamine represented by formula (1)wherein A is a phenylene group or a cyclohexylene group.6: The process according to claim 1 , {'br': None, 'H2N—(CH2CH2NH)n-H\u2003\u2003(2),'}, 'wherein the polyamine is a polyamine represented by formula (2)wherein n is an integer of from 1 to 5.7: The process according to claim 1 ,wherein the polyamine is a cyclic aliphatic polyamine having 9 or more carbon atoms and 2 or more amino groups in a molecule thereof as well as 3 or more active hydrogen atoms derived from amino groups.8: The process according to claim 7 ,{'b': 4', '3, 'wherein the cyclic aliphatic polyamine is menthenediamine, isophoronediamine, diaminodicyclohexyl methane, bis(-amino--methylcyclohexyl)methane, N-aminomethyl piperazine, or norbornanediamine.'}9: The process according to claim 1 ,wherein the ...

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Номер записи: 31

21-11-2013 дата публикации

PROCESS FOR PREPARATION OF SUBSTITUTED P-AMINOPHENOL

Номер: US20130310597A1

Автор: BUSACCA Carl Alan, ERIKSSON Magnus C., Xu Jinghua, ZENG Xingzhong

Принадлежит: BOEHRINGER INGELHEIM INTERNATIONAL GMBH

The present invention is related to a process of preparing substituted p-aminophenol compound of formula (I) or a salt thereof, 2. The process of claim 1 , wherein the suitable solvent in scheme 1 of Step A is 2-methyltetrahydrofuran (MeTHF).3. The process of claim 1 , wherein the isolation procedure of Step A comprise cooling the reaction mixture to room temperature after the reaction is complete claim 1 , quenching the reaction by adding water claim 1 , adjusting the pH of the reaction mixture to be acidic claim 1 , separating the organic layer from the aqueous layer of the reaction mixture claim 1 , washing the organic layer with water claim 1 , reducing the volume of organic layer to form a residue of the crude product claim 1 , stirring the residue of the crude product in a solvent to form a slurry suspension claim 1 , filtering the slurry suspension claim 1 , and drying the solid to provide the compound of formula (III).4. The process of claim 1 , wherein the suitable solvent to form the acid chloride intermediate in scheme 2 of Step B is 2-methyltetrahydrofuran (MeTHF).5. The process of claim 1 , wherein the suitable amount of oxalyl chloride in Step B is 1-1.5 equivalents compared to the amount of the compound of formula (III).6. The process of claim 1 , wherein the alcohol of Step B is anhydrous methanol claim 1 , or ethanol.7. The process of claim 1 , wherein yield of the Step B is at least about 92%.8. The process of claim 1 , wherein the isolation procedure of Step B comprises adjusting the pH of the reaction mixture to be neutral by adding basic reagents into the reaction mixture after the reaction is complete claim 1 , separating the organic layer from the aqueous layer of the reaction mixture claim 1 , reducing the volume of organic layer to form a residue of the crude product claim 1 , stirring the residue of the crude product in a solvent to form a slurry suspension claim 1 , filtering the slurry suspension claim 1 , and drying the solid to provide ...

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Номер записи: 32

05-12-2013 дата публикации

PROCESSES FOR THE PREPARATION OF DI-(2-AMINOETHYL) FORMAL, DI-(3-AMINOPROPYL) FORMAL, AND RELATED MOLECULES

Номер: US20130324764A1

Автор: Pastine Stefan J.

Принадлежит:

Disclosed herein are hardeners for use in making cleavable epoxy compositions, including compositions wherein components in contact with epoxy composition can be recovered, as well as methods of making such hardeners. 2. The process of chemical synthesis of claim 1 , wherein 2 molar equivalents of the compound of formula IX and 1 molar equivalent of paraformaldehyde are used.3. The process of chemical synthesis of claim 1 , wherein the catalytic hydrogenation occurs under aqueous reaction conditions.4. The process of chemical synthesis of claim 1 , wherein the catalytic hydrogenation uses a catalyst including claim 1 , as an active component claim 1 , a metal selected from the group consisting of Ru claim 1 , Rh claim 1 , Pd claim 1 , and Pt.5. The process of chemical synthesis of claim 1 , wherein the catalytic hydrogenation uses a catalyst including claim 1 , as an active component claim 1 , a metal selected from the group consisting of Cu claim 1 , Cr claim 1 , Co claim 1 , Ni claim 1 , Fe claim 1 , Raney catalysts and chromite catalysts.6. The process of chemical synthesis of claim 1 , wherein the catalytic hydrogenation uses a catalyst including claim 1 , as an active component claim 1 , a bimetallic catalyst comprising one or more transition metals and/or noble metals.7. The process of chemical synthesis of claim 1 , wherein the catalytic hydrogenation is conducted in liquid or vapor phase.8. The process of chemical synthesis of claim 1 , wherein the catalytic hydrogenation is conducted at temperatures between 20° C. and 200° C.9. The process of chemical synthesis of claim 1 , wherein the catalytic hydrogenation is conducted at hydrogen pressure between 1 and 1000 atmospheres.10. The process of chemical synthesis of claim 1 , wherein the catalytic hydrogenation is conducted at a temperate between 60° C. and 150° C.11. The process of chemical synthesis of claim 1 , wherein the catalytic hydrogenation is conducted under hydrogen pressure between 10 atmospheres ...

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Номер записи: 33

12-12-2013 дата публикации

Process for Preparing Piperazine

Номер: US20130331573A1

Автор: Abel Ulrich, Bou Chedid Roland, Challand Nina, Dostalek Roman, Jödecke Michael, Melder Johann-Peter, Stein Bernd

Принадлежит:

Process for preparing piperazine of the formula I 134-. (canceled)36. The process according to claim 35 , wherein the catalytically active mass of the catalyst claim 35 , prior to its reduction with hydrogen claim 35 , comprises in the range from 0.4 to 4.0% by weight of oxygen-containing compounds of tin claim 35 , calculated as SnO.37. The process according to claim 35 , wherein the catalytically active mass of the catalyst claim 35 , prior to its reduction with hydrogen claim 35 , comprises in the range from 0.6 to 3.0% by weight of oxygen-containing compounds of tin claim 35 , calculated as SnO.38. The process according to claim 35 , wherein the catalytically active mass of the catalyst claim 35 , prior to its reduction with hydrogen claim 35 , comprises in the range from 5.0 to 35% by weight of oxygen-containing compounds of cobalt claim 35 , calculated as CoO.39. The process according to claim 35 , wherein the catalytically active mass of the catalyst claim 35 , prior to its reduction with hydrogen claim 35 , comprises in the range from 10 to 30% by weight of oxygen-containing compounds of cobalt claim 35 , calculated as CoO.40. The process according to claim 35 , wherein the catalytically active mass of the catalyst claim 35 , prior to its reduction with hydrogen claim 35 , comprises in the range from{'sub': 2', '3, '15 to 80% by weight of oxygen-containing compounds of aluminum, calculated as AlO,'}1.0 to 20% by weight of oxygen-containing compounds of copper, calculated as CuO, and5.0 to 35% by weight of oxygen-containing compounds of nickel, calculated as NiO.41. The process according to claim 35 , wherein the catalytically active mass of the catalyst claim 35 , prior to its reduction with hydrogen claim 35 , comprises in the range from{'sub': 2', '3, '30 to 70% by weight of oxygen-containing compounds of aluminum, calculated as AlO, 2.0 to'}18% by weight of oxygen-containing compounds of copper, calculated as CuO, and10 to 30% by weight of oxygen- ...

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Номер записи: 34

12-12-2013 дата публикации

PROCESS FOR THE DIRECT AMINATION OF ALCOHOLS USING AMMONIA TO FORM PRIMARY AMINES BY MEANS OF A XANTPHOS CATALYST SYSTEM

Номер: US20130331580A1

Автор: Beller Matthias, Deutsch Jens, Haas Thomas, Haberland Juergen, Imm Sebastian, Klasovsky Florian, Koeckritz Angela, Martin Andreas, Pfeffer Jan Christoph, Tacke Thomas

Принадлежит: EVONIK DEGUSSA GmbH

The present invention relates to a chemocatalytic liquid-phase process for the direct one-stage amination of alcohols to primary amines by means of ammonia in high yields using a catalyst system containing at least one transition metal compound and a xantphos ligand. 2. The process according to claim 1 ,wherein{'sup': 1', '2', '3', '4, 'sub': 3', '2, 'R=R=R=R=phenyl, and A=—C(CH)—.'}3. The process according to claim 1 ,whereinthe xantphos ligand is carbonylchlorohydrido[9,9-dimethyl-4,5-bis(diphenylphosphino)xantheno]ruthenium(II)].4. The process according to claim 1 ,whereinthe alcohol is an aliphatic, linear ω-hydroxycarboxylic acid having a carbon chain comprising at least 8 carbon atoms.5. The process according to claim 1 ,whereinthe alcohol has a concentration of from 0.1 to 1000 mmol/l, based on the fluid phase.6. The process according to claim 1 ,wherein the contacting comprises contacting with liquid or supercritical ammonia, with a solution of ammonium salts in a solvent, or both.7. The process according to claim 1 ,wherein in the contacting,the ammonia has a molar ratio to hydroxyl groups in the alcohol of at least 5:1.8. The process according to claim 1 ,wherein the contacting is carried out at a pressure of from 1 to 1000 bar.9. The process according to claim 1 ,wherein the contacting is carried out in a temperature range of from 80 to 220° C.10. The process according to claim 1 ,whereina volume ratio of a liquid phase to a gas phase in the contacting is greater than or equal to 0.05.11. The process according to claim 1 ,wherein the process is carried out in an absence of hydrogen.12. The process according to claim 1 , wherein the alcohol has a concentration of from 0.1 to 100 mmol/l based on the fluid phase.13. The process according to claim 1 , wherein the alcohol has a concentration of from 0.1 to 10 mmol/l based on the fluid phase.14. The process according to claim 1 , wherein in the contacting claim 1 , the ammonia has a molar ratio to hydroxyl ...

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Номер записи: 35

19-12-2013 дата публикации

Process for the Synthesis of Aminobiphenylene

Номер: US20130338369A1

Автор: Heinrich Markus, Pratsch Gerald

Принадлежит: BASF SE

The present invention relates to a process for the synthesis of 2-aminobiphenylene and derivatives thereof by reacting a benzene diazonium salt with an aniline compound under basic reaction conditions. 127-. (canceled)31. The process of claim 28 , wherein the reaction is performed at a pH of 9.1 or greater32. The process of claim 28 , wherein the reaction is performed in the presence of at least one solvent.33. The process of claim 32 , wherein the solvent is an aqueous solvent.34. The process of claim 28 , wherein the reaction is performed in the presence of water and of at least one base.35. The process of claim 34 , wherein the base is selected from the group consisting of alkali metal hydroxides claim 34 , alkaline earth metal hydroxides claim 34 , alkali metal carbonates and alkali metal phosphates claim 34 , and is preferably sodium hydroxide or potassium hydroxide.36. The process of claim 28 , wherein the reaction is performed within the temperature range from 50 to 130° C.37. The process of claim 28 , wherein the compound of the formula 1 or the compound of the formula 2 or both compounds 1 and 2 are used in the reaction dispersed in an alkaline medium.38. The process of claim 37 , wherein the pH of the alkaline medium is at least 9.1.39. The process of claim 28 , wherein claim 28 , in a first step claim 28 , a compound of the formula 1 is reacted with a base in aqueous medium and claim 28 , in a second step claim 28 , the dispersion obtained is added to the compound of the formula 2.40. The process of claim 39 , wherein the pH of the dispersion obtained is at least 9.1.41. The process of claim 39 , wherein the compound 2 claim 39 , prior to addition of the dispersion claim 39 , is brought to a temperature of 50 to 130° C.42. The process of claim 28 , wherein the compound of the formula 2 is initially charged in an alkaline medium and the compound of the formula 1 is added.43. The process of claim 42 , wherein the compound of the formula 2 is initially ...

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Номер записи: 36

19-12-2013 дата публикации

Process for Preparing Substituted 3-(1-amino-2-methylpentane-3-yl)phenyl Compounds

Номер: US20130338399A1

Автор: Buschmann Helmut Heinrich, HOLENZ Joerg

Принадлежит: GRUENENTHAL GmbH

A process for the preparation of substituted 3-(1-amino-2-methylpentane-3-yl)phenyl compounds which has advantages over conventional processes with respect to higher conversions and yields, flexibility, a shorter overall route, environmentally acceptable conditions, influence of stereoselectivity such as diastereoselectivity in a targeted manner and at least partial suppression of the formation of undesired side-products and/or undesired stereoisomers, in particular undesired diastereomers. 2. A process according to claim 1 , wherein said compound is in the form of an isolated stereoisomer.3. A process according to claim 2 , wherein said compound is in the form of an isolated enantiomer or diastereomer.4. A process according to claim 1 , wherein said compound is in the form of a mixture of stereoisomers in any mixing ratio.5. A process according to claim 4 , wherein said compound is in the form of a racemic mixture of stereoisomers.6. A process according to claim 1 , wherein in alternative A:the hydrogenation step (a-I) is effected via heterogeneous or homogeneous catalysis in the presence of hydrogen, andthe reduction step (a-II) is carried out by employing at least one metal hydride, at least one borane or hydrogen in combination with a catalyst as reducing agent.7. A process according to claim 1 , wherein in alternative A:the hydrogenation step (a-I) is effected via heterogeneous catalysis in the presence of hydrogen by employing at least one catalyst selected from the group consisting of Raney nickel, palladium, palladium on carbon, platinum, platinum on carbon, ruthenium on carbon and rhodium on carbon, andthe reduction step (a-II) is carried out by employing as reducing agent at least one metal hydride selected from the group consisting of lithium aluminium hydride, sodium borohydride, diisobutyl aluminium hydride, and selectrides.9. A process according to claim 1 , wherein alternative A further comprises a step (a-V) in which the compound according to formula ...

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Номер записи: 37

19-12-2013 дата публикации

PROCESS FOR THE PRODUCTION OF AMINO ALCOHOLS

Номер: US20130338401A1

Автор: Tjosas Freddy

Принадлежит: BORREGAARD AS

The present invention relates to a process for the manufacture of APD and N-alkyl-APD wherein 1-CPD is reacted with aqueous ammonium or aqueous alkyl-amine under alkaline conditions and where the process is conducted in a continuous manner in a reactor comprising a tubular reactor wherein at least two reaction zones are established. 1. Process for the manufacture of APD and N—C-C-alkyl-APD wherein comprising reacting 1-CPD is reacted with aqueous ammonium or aqueous C-C-alkyl-amine under alkaline conditions , characterized in that wherein the process is conducted in a continuous manner in a reactor comprising a tubular reactor , and wherein at least two reaction zones are established.2. Process of wherein the tubular reactor is a microreactor or a millireactor3. Process of claim 1 , wherein the reactor contains two separate reaction zones.4. Process of claim 1 , wherein a first reaction zone is adapted for the formation of glycidol by the reaction of 1-CPD in alkaline conditions.5. Process of claim 4 , wherein at reactor inlets of the first reaction zone claim 4 , 1-CPD and base are injected through separate inlets into a mixing zone at injection speeds sufficient to ensure thorough mixing of the reactants.6. Process of claim 4 , wherein alkali claim 4 , is added to keep the pH of the mixture between 10 and 13.7. Process of claim 4 , wherein the temperature in the first reaction zone of the tubular reaction is above ambient temperature.8. Process of claim 7 , wherein the temperature in the first reaction zone of the tubular reactor is up to about 60° C.9. Process of claim 7 , wherein the temperature in the first reaction zone of the tubular reactor is from about 35° C. to about 45° C.10. Process of claim 1 , wherein a second reaction zone is adapted for the formation of APD or N—C-C-alkyl-APD by the reaction of glycidol with ammonium or with C-C-alkyl-amine.11. Process of wherein at least 2 moles of ammonium or C-C-alkylamine are added per mole 1-CPD.12. Process of ...

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Номер записи: 38

26-12-2013 дата публикации

Polyetheramine Macromonomers Comprising Two Neighboring Hydroxyl Groups And Their Use For Producing Polyurethanes

Номер: US20130345386A1

Автор: Muenter Juergen, POELLMANN Klaus

Принадлежит: Clariant Finance (BV I) Limited

The object of the invention are compounds of the formula (2) wherein Ris H, methyl or ethyl, Ris C- to Calkyl, A is a C- to Calkylene group, m is number from 10 to 400, n is 1, 2, 3, 4, or 5, a method for their production and their use in the production of polyurethane prepolymers. 17.-. (canceled)13. (canceled)14. (canceled)15. The process as claimed in claim 8 , wherein the alkylene oxide is ethylene oxide.16. The process as claimed in claim 8 , wherein the dihydroxyalkylamino group is a dihydroxyethylamino group.17. A polyurethane prepolymer made in accordance with the process of .18. A polyurethane polymer made in accordance with the process of .19. A polyurethane prepolymer made in accordance with the process of .20. A polyurethane polymer made in accordance with the process if . The present invention relates to Ω-(alkoxy)-α-N,N-dihydroxyalkylaminopoly-alkylene glycols, and to their use for producing water-dispersible polyurethanes.On account of their high resistance and simple application, polyurethane systems have acquired a broad application field in the paint, (surface) coating and textile industry sector. For reasons of environmental protection and occupational protection, in the recent past primarily solvent-free, water-dispersed polyurethane systems have been developed.The production of aqueous polyurethane dispersions has been known for many years and is described in detail in a large number of publications (e.g. Houben-Weyl, Methoden der Organischen Chemie [Methods of organic chemistry], Volume E20, Part I, pp. 1659-1681; D. Dieterich, Prog. Org. Coat. 1981, 9, 281-330; J. W. Rosthauser, K. Nachtkamp, Journal of Coated Fabrics 1986, 16, 39-79; R. Arnoldus, Surf. Coat. 1990, 3 (Waterborne Coat.), 179-198).Aqueous polyurethane dispersions consist of polyurethane polymers or polyurethane-polyurea polymers which include both urethane groups and also urea groups and are accessible by polyaddition reactions of polyols, polyisocyanates and polyamines. Firstly ...

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Номер записи: 39

09-01-2014 дата публикации

METHOD FOR PRODUCTION OF F-18 LABELED AMYLOID BETA LIGANDS

Номер: US20140012032A1

Автор: Ackermann Uwe, Berndt Mathias, LEHMANN Lutz

Принадлежит: PIRAMAL IMAGING SA

This invention relates to methods, which provide access to F-18 labeled stilbene derivatives. 2. A compound according to claim 1 ,Wherein PG is selected from the group consisting of:a) Boc,b) Trityl andc) 4-Methoxytrityl3. A compound according claim 1 ,whereinArylsulfonyloxy is selected from the group consisting ofp-Toluenesulfonyloxy, 4-Cyanophenylsulfonyloxy, 4-Bromophenylsulfonyloxy, 4-Nitrophenylsulfonyloxy, 2-Nitrophenylsulfonyloxy, 4-Isopropyl-phenylsulfonyloxy, 2,4,6-Triisopropyl-phenylsulfonyloxy, 2,4,6-Trimethylphenylsulfonyloxy, 4-tert-Butyl-phenylsulfonyloxy, 4-Adamantylphenylsulfonyloxy and 4-Methoxyphenylsulfonyloxy.7. A method according to claim 5 , wherein the method is a fully automated method.9. A kit according to claim 8 ,whereinPG is selected from the group comprising:a) Boc,b) Trityl andc) 4-Methoxytrityl10. A kit according to claim 8 ,WhereinArylsulfonyloxy is selected from the group comprising:a) p-Toluenesulfonyloxyb) (2-Nitrophenyl)sulfonyloxy,c) (4-Cyanophenyl)sulfonyloxyd) (4-Bromophenyl)sulfonyloxy,e) (4-Adamantylphenyl)sulfonyloxy.11. A kit comprising at least one sealed container containing a compound as defined by . This invention relates to compounds and methods, which provide access to F-18 labeled stilbene derivatives.4-[(E)-2-(4-{2-[2-(2-fluoroethoxy)ethoxy]ethoxy}phenyl)vinyl]-N-methylaniline has been labeled with [F-18]fluoride and is claimed by patent application WO2006066104 and members of the corresponding patent family.The usefulness of this radiotracer for the detection of Aβ plaques have been reported in the literature (W. Zhang et al., Nuclear Medicine and Biology 32 (2005) 799-809; C. Rowe et al., Lancet Neurology 7 (2008) 1-7).The synthesis of 4-[(E)-2-(4-{2-[2-(2-[F-18]fluoroethoxy)ethoxy]ethoxy}phenyl)-vinyl]-N-methylaniline has been described before:Very recently, further methods have been described:So far, one-pot radiolabelings have been performed using a mesylate precursor. It is know, that for F-18 labeling of ...

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Номер записи: 40

06-02-2014 дата публикации

BROMFENAC ORGANIC SALTS AND PREPARATION METHOD, COMPOSITION AND USE THEREOF

Номер: US20140039056A1

Автор: Liu Jidong, Tang Hai, Wang Jiuliang, Yang Yuchun

Принадлежит: SHENYANG XINGQI PHARMACEUTICAL CO., LTD.

Provided are bromfenac organic salts and preparation method, composition and use thereof. The bromfenac organic salt has the structure as shown in the following Formula I, wherein A represents an organic base. Also provided are a method for the preparation of the bromfenac organic salt, a composition comprising the bromfenac organic salts, a use of the bromfenac organic salts or the composition thereof in manufacture of a medicament for treatment and/or prophylaxis of an inflammation or for analgesia, and a method for treatment and/or prophylaxis of an inflammation or for analgesia. 3. A method for preparing the bromfenac organic salt according to claim 1 , comprising the steps:1) dissolving bromfenac in an organic solvent, heating to dissolve, then adding an organic base in equimolar amount, stirring until the end of reaction;2) concentrating and evaporating the reaction solution to dry to obtain a light yellow or orange yellow solid; and3) recrystallizing the solid obtained in step 2) to obtain the bromfenac organic salt.4. The method according to claim 3 , wherein said organic solvent in step 1) is one or more selected from the group consisting of methanol claim 3 , ethanol claim 3 , acetone claim 3 , n-butanol and toluene; and said organic base is a nitrogen-containing organic base.5. The method according to claim 3 , wherein the temperature of heating in step 1) is 25-80° C.6. The method according to claim 3 , wherein the time for stirring and reacting in step 1) is 0.5-2 hours.7. The method according to claim 3 , wherein the recrystallization in step 3) is performed at 0° C. or below.8. The method according to claim 3 , further comprising step 4): vacuum drying the crystal obtained by recrystallizing.9. A composition claim 1 , comprising the bromfenac organic salt according to .10. (canceled)11. A method for treatment and/or prophylaxis of an inflammation or for analgesia claim 1 , comprising a step of administering an effective amount of the bromfenac organic ...

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Номер записи: 41

13-03-2014 дата публикации

ONO PINCER LIGANDS AND ONO PINCER LIGAND COMPRISING METAL COMPLEXES

Номер: US20140073800A1

Автор: "OREILLY MATTHEW", JAN MUHAMMAD TARIQ, VEIGE ADAM STEVEN

Принадлежит: UNIVERSITY OF FLORIDA RESEARCH FOUNDATION, INC.

Embodiments of the invention are directed to ONO pincer ligands that can be in a trianionic, protonated or protonated equivalent form. The ONO pincer ligand can be combined with a transition metal comprising compound to form an ONO pincer ligand comprising transition metal complex. By choice of the ONO pincer ligand structure, the steric and electronic properties of the transition metal complexes therefrom can be controlled. The ONO pincer ligands comprise a central nitrogen atom that is disubstituted with a pair of three atom comprising bridges where the three atoms are three sphybridized carbons or the three atoms are a pair of sphybridized carbons and an sphybridized carbon or silicon. 5. A method of preparing an ONO pincer ligand precursor according to claim 1 , comprising condensing a nucleophilic oxygen or nucleophilic nitrogen comprising compound with an electrophilic carbon comprising compound further comprising the bridge structure of the resulting ONO pincer ligand.6. A trianionic ONO pincer ligand comprising transition metal complex comprising:{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, 'at least one ONO trianionic pincer ligand derived from the ONO trianionic pincer ligand precursor of ; and'}a transition metal from group III through group X of the periodic table.7. The trianionic ONO pincer ligand comprising transition metal complex of claim 6 , wherein the transition metal is an early transition metal complex from group III through group VI.18. The method of preparing an ONO pincer ligand comprising transition metal complex of claim 17 , wherein the precursor metal compound further comprises a metal alkylidyne claim 17 , further comprising adding the OH or NH of the ONO pincer ligand precursor across the metal alkylidyne to form the anionic ONO pincer ligand comprising metal complex. This application is a continuation-in-part of International Patent Application No. PCT/US2012/037302, filed May 10, 2012, which claims the benefit of U.S. ...

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Номер записи: 42

20-03-2014 дата публикации

High-yield process for the synthesis of urea

Номер: US20140081046A1

Автор: Alessandro Gianazza, Lino Carlessi

Принадлежит: Saipem Spa

A process for the direct synthesis of urea from ammonia and carbon dioxide at high pressures and temperatures, with the formation of ammonium carbamate as intermediate, comprising a decomposition step of the ammonium carbamate and stripping of the gases formed, operating substantially at the same pressure as the synthesis step, wherein the recycled liquid streams are fed, at least partially, to the same decomposition and stripping step after being preheated by heat exchange with a stream included in the high-pressure synthesis cycle.

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Номер записи: 43

03-04-2014 дата публикации

Process

Номер: US20140094625A1

Автор: Sedelmeier Gottfried

Принадлежит: NOVARTIS AG

The present invention relates to improved processes for the production of 2-amino-2-[2-(4-Calkyl-phenyl)ethyl]propane-1,3-diols, and to compounds for use therein. 7. A process according to claim 1 , wherein Ris n-hexyl.12. The process of claim 2 , which is performed on a continuous flow. The present invention relates to processes for the production of 2-amino-2-[2-(4-C-alkyl-phenyl)ethyl]propane-1,3-diols, and to compounds for use therein.2-Amino-2-[2-(4-C-alkyl-phenyl)ethyl]propane-1,3-diols are disclosed in EP-A-1627406 the relevant disclosure of which is incorporated herein by reference. On the basis of observed activity, the compounds have been found to be useful as immunosuppressants. Accordingly, the compounds may be useful in the treatment or prevention of acute allograft rejection, autoimmune diseases or xenograft rejection. A particular compound of this type is FTY720, i.e. 2-amino-2-[2-(4-octylphenyl)ethyl]propane-1,3-diol, which has the following structure:FTY720 has been found to be useful in the prevention of autoimmune diseases, such as multiple sclerosis. FTY720 is the first-in-class sphingosine 1-phosphate (SIP) receptor modulator which has been effective in clinical trials for Multiple Sclerosis.WO 00/27798 discloses various processes for the preparation of 2-amino-2-[2-(4-C-alkyl-phenyl)ethyl]propane-1,3-diols. Some of these processes are illustrated in the reaction scheme below in relation to the production of FTY720, using the reference numerals given in the publication:The above processes involve formation of intermediate 18 via acylation of compound 16. However, the acylation process results in a mixture of ortho-, meta- and para-substituted products. None all these products have biological activity. There is a need for a processes for producing 2-amino-2-[2-(4-C-alkyl-phenyl)ethyl]propane-1,3-diols, in particular FTY720 and salts thereof, which have improved regioselectivity for the para-position of the benzene ring.Furthermore the above ...

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Номер записи: 44

03-04-2014 дата публикации

FLUIDIC CHANNEL COATED WITH METAL CATALYSTS AND DEVICES AND METHODS RELATING THERETO

Номер: US20140094626A1

Автор: CHALLA Siva Sai Ramana Kumar

Принадлежит:

The invention provides a method for coating fluidic channels, particularly millifluidic channels, with a catalyst coating having controlled dimensions and morphology, and methods for preparing such channels, and devices that can be used in combination with the channels. The invention further provides portable, hand-held millifluidic devices applicable for a wide variety of uses including molecular reduction reactions, in situ material characterization, in situ reaction catalysis characterization, in situ reaction mechanism characterization, nanomaterial synthesis, nanostructured metal and metal oxide growth and coating of channels, continuous flow cell culturing, enzymatic catalysis, biomolecular catalysis, combinatorial chemistry, reactions involving homogeneous catalysts bound to channel walls, peptide synthesis, nucleic acid synthesis, synthesis of pharmaceutical intermediates, biofunctionalization of nanomaterials or a combination thereof. 1. A hand-held millifluidic device comprising:a removable chip having one or more millifluidic supply channels connecting to a primary channel wherein the primary channel is coated with catalytic structures having a controlled size and morphology;at least one pump connected to a supply channel or the primary channel;a flow controller; anda power source;wherein the chip is disposable or reusable.2. The device of wherein the catalytic structures have diameters of 0.01 microns to about 5 claim 1 ,000 microns and morphological features in the range of 1 nm to about 500 nm.3. The device of further comprising one or more in situ time resolved probes.4. The device of wherein the primary channel is greater than about 100 m in length and greater than 10 mm in width.5. The device of wherein the primary channel configuration is straight claim 1 , serpentine claim 1 , irregular serpentine claim 1 , zig zag claim 1 , spiral claim 1 , or a combination thereof claim 1 , optionally in combination with one or more chambers.6. The device of ...

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Номер записи: 45

10-04-2014 дата публикации

PROCESS FOR PREPARATION OF SUCCINYLCHOLINE CHLORIDE

Номер: US20140100385A1

Автор: Arulmoli Thangavel, DAS Gautam Kumar, MANJATHURU Mahalinga, MAYEKAR Anil Narayan, VASUDEVA Pejakala Kakrannaya

Принадлежит: Sequent Scientific Limited

The present invention relates to a process for the preparation of succinylcholine chloride, a pharmaceutically active compound used as skeletal muscle relaxant which comprises condensing succinic anhydride with N,N-diemthylaminoethanol using a catalyst in presence of a solvent to form bis[2-(dimethylamino)ethyl]succinate; in situ purifying the bis[2-(dimethylamino)ethyl]succinate using a base; reacting pure bis[2-(dimethylamino)ethyl]succinate with methyl chloride gas using an alcohol; and purifying the obtained crude succinylcholine chloride using water and alcohol. 2. The process of claim 1 , wherein the catalyst in step a) is selected from the group consisting of mineral acids claim 1 , trifluoro acetic acid claim 1 , and p-toluene sulfonic acid (PTSA).3. The process of claim 1 , wherein the acid catalyst in step a) is p-toluene sulfonic acid.4. The process of claim 1 , wherein the acidic resin is an amberlite.5. The process of claim 1 , wherein the solvent in step a) is an inert organic solvent selected from the group consisting of toluene claim 1 , benzene claim 1 , and xylene.6. The process of claim 1 , wherein the solvent in step a) is toluene.7. The process of claim 1 , wherein the condensation in step a) is carried out at about 110-120° C.8. The process of claim 1 , wherein the base used in step b) is an alkali metal carbonate or alkali metal bicarbonate or an organic base.9. The process of claim 1 , wherein the base used in step b) is potassium carbonate.10. The process of claim 1 , wherein the reaction in step c) is carried out at about 55-65° C.11. The process of claim 1 , wherein step c) occurs in a solvent.12. The process of claim 11 , wherein the solvent is isopropanol.13. The process of claim 1 , the alcohol in step d) is isopropanol. This application claims the priority of Indian Patent Application No. 2938/MUM/2012, filed Oct. 8, 2012, which is incorporated herein by reference.The present invention relates to a novel process for the preparation of ...

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Номер записи: 46

10-04-2014 дата публикации

POLYETHER COMPOUND, CURING AGENT USING THE POLYETHER COMPOUND, AND PRODUCING METHOD OF THE POLYETHER COMPOUND

Номер: US20140100390A1

Автор: AMAO Akihito, KITAGAWA Hirotaka

Принадлежит: FUJIFILM Corporation

Disclosed is a polyether compound which is useful as a curing agent or the like, a curing agent using the compound and a producing method of the compound. The polyether compound of the present invention is represented by the following general formula (1). 2. The polyether compound according to claim 1 , wherein Rrepresents a hydrogen atom in the general formula (1).3. The polyether compound according to claim 1 , wherein Rrepresents a hydrogen atom and Rrepresents —C(═O)—C(R)═CHin the general formula (1).4. A curing agent using the polyether compound according to .5. A curing agent using the polyether compound according to .6. A curing agent using the polyether compound according to . 1. Field of the InventionThe present invention relates to a polyether compound, a curing agent using the polyether compound and a producing method of the polyether compound.2. Description of the Related ArtAs a raw material of various kinds of polymers and curable resin compositions, a polymerizable compound which is polymerized and cured by imparting energy such as heat and light, is widely used for industrial uses such as coating materials, paints, printing inks, adhesive agents and resist materials.For example, an epoxy resin (an epoxy compound) is used in various fields such as an adhesive agent for civil engineering and constructions, a sealing agent for semiconductors, an insulating material for printed circuit boards, mold devices for high voltage power, or the like, paints for cans, automobiles, or the like due to its excellent characteristics and diversity.It is possible to improve the characteristics of an obtained molded body (a cured product) by using a polymerizable compound. For example, by the compound being polymerized to be a cured film by heating after an image is formed by using inks or paints containing a polymerizable compound which is cured by heat, an image which has an excellent weather resistance and durability can be created.Curing of the polymerizable ...

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Номер записи: 47

03-01-2019 дата публикации

IMPROVED METHOD FOR SYNTHESISING PARTIALLY N-HYDROXYETHYLATED TERTIARY 1,6-HEXANEDIAMINES

Номер: US20190002392A1

Автор: Delfort Bruno, Grandjean Julien

Принадлежит: IFP ENERGIES NOUVELLES

The invention relates to a synthesis method for at least one nitrogen compound belonging to the family of partly N-hydroxyethylated tertiary 1,6-hexanediamines with general formula (I) as follows: 3) A method as claimed in claim 1 , wherein the first precursor compound is 1 claim 1 ,6-hexanediamine and the second precursor compound 2 PET-3256 is ethylene oxide claim 1 , said method comprising:a first reaction step between the 1,6-hexanediamine and the ethylene oxide so as to form at least one intermediate compound selected from the list including N-(2-hydroxyethyl)-1,6-hexanediamine, N,N′-di(2-hydroxyethyl)-1,6-hexanediamine, N,N-di(2-hydroxyethyl)-1,6-hexanediamine and N,N,N′-tri(2-hydroxyethyl)-1,6-hexane-diamine;a second step of methylation of the primary or secondary amine functions of said at least one intermediate compound so as to form at least one compound according to general formula (I).4) A method as claimed in claim 3 , wherein the second methylation step is carried out by reaction between said intermediate compound claim 3 , formaldehyde and hydrogen in the presence of a hydrogenation catalyst claim 3 , or by reaction between said intermediate compound claim 3 , formaldehyde and formic acid according to the Eschweiler-Clarke reaction.5) A method as claimed in claim 3 , wherein the residual 1 claim 3 ,6-hexanediamine that has not reacted at the end of the first reaction step is recycled to said first reaction step claim 3 , after separation by distillation of said 1 claim 3 ,6-hexanediamine from said at least one intermediate compound.6) A method as claimed in claim 3 , wherein the molar ratio of ethylene oxide to 1 claim 3 ,6-hexanediamine is less than or equal to 3/1 claim 3 , and preferably less than or equal to 2.5/1.7) A method as claimed in claim 3 , further comprising claim 3 , at the end of the first reaction step claim 3 , at least one separation step claim 3 , preferably by distillation claim 3 , of at least one intermediate compound so as to ...

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Номер записи: 48

12-01-2017 дата публикации

TWO-STEP PROCESS FOR PREPARING 3-SUBSTITUTED PHENYLALKYLAMINES

Номер: US20170008832A1

Автор: Liao Subo, Teramura Doug

Принадлежит:

Processes for preparing 3-substituted phenylalkylamines comprising reacting a phenyl boronic compound with an α-β unsaturated carbonyl-containing compound via an asymmetric 1,4-addition reaction, followed by reductive alkylation. The processes may be useful in the synthesis of tapentadol. 2. The process of claim 1 , wherein R is hydrogen claim 1 , C-Calkenyl claim 1 , substituted C-Calkenyl claim 1 , aryl claim 1 , substituted aryl claim 1 , or aryl(C-C)alkyl; Ris hydrogen claim 1 , alkyl claim 1 , or substituted alkyl; Rand Rare independently alkyl or substituted alkyl; R claim 1 , R claim 1 , R claim 1 , and Rare independently hydrogen claim 1 , alkyl claim 1 , substituted alkyl claim 1 , hydroxyl claim 1 , alkoxy claim 1 , substituted alkoxy claim 1 , aryl claim 1 , substituted aryl claim 1 , alkylaryl claim 1 , or substituted alkylaryl; Rand Rare independently alkyl or substituted alkyl; and Rand Rare independently hydrogen claim 1 , alkyl claim 1 , aryl claim 1 , alkylaryl claim 1 , or organoborane.3. The process of claim 2 , wherein R is hydrogen or benzyl; Ris hydrogen; Rand Rare independently C-Calkyl; each of R claim 2 , R claim 2 , R claim 2 , and Ris hydrogen; and Rand Rare independently C-Calkyl.4. The process of claim 1 , wherein the compound of Formula (I) is 3-hydroxyphenylboronic acid claim 1 , 3-hydroxyphenyl trifluoroborate claim 1 , 3-hydroxyphenylboronic acid pinacol ester claim 1 , 3-hydroxyphenylboronic ester claim 1 , derived from 3-hydroxyphenylboroxine claim 1 , 3-benzyloxyphenylboronic acid claim 1 , 3-benzyloxyphenyl trifluoroborate claim 1 , 3-benzyloxyphenylboronic acid pinacol ester claim 1 , 3-benzyloxyphenylboronic ester claim 1 , or is derived from 3-benzyloxyphenylboroxine.5. The process of claim 1 , wherein the compound of Formula (I) and the compound of Formula (IV) are present at a molar ratio of about 1:0.5 to about 1:6.0.6. The process of claim 1 , wherein the transition metal catalyst comprises rhodium claim 1 , palladium ...

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Номер записи: 49

14-01-2016 дата публикации

A PROCESS FOR THE PREPARATION OF 2-AMINO-1,3-PROPANE DIOL COMPOUNDS AND SALTS THEREOF

Номер: US20160009634A1

Автор: Aswathanarayanappa Chandrashekar, CHANDREGOWDA Dharshan Jakkali, Duvva Chandrasekhar, Kumar Kothakonda Kiran, PULLELA Venkata Srinivas

Принадлежит:

The present disclosure relates to processes for the preparation of 2-amino-1,3-propane diol compounds and their hydrochloride salts. Particularly, the present disclosure relates to processes for synthesizing 2-amino-2-(2-(4-octylphenyl)ethyl)-1,3-propanediol and its hydrochloride salt 2-amino-2-(2-(4-octylphenyl)ethyl)-1,3-propanediol hydrochloride respectively. The said process is safe, commercially feasible for large-scale synthesis and has improved efficacy along with many other advantages. The present disclosure also relates to the novel polymorphs of 2-amino-1,3-propane diol compound and its hydrochloride salt, where in 2-amino-1,3-propane diol compound is 2-amino-2-(2-(4-octylphenyl)ethyl)-1,3-propanediol, and its hydrochloride salt is 2-amino-2-(2-(4-octylphenyl)ethyl)-1,3-propanediol hydrochloride. 2. The process as claimed in claim 1 , wherein the reaction of step (a) is carried out in presence of solvent selected from a group comprising toluene claim 1 , xylene claim 1 , heptanes claim 1 , hexanes claim 1 , diethyl ether claim 1 , methyl tertiary butyl ether and tetrahydrofuran or any combination thereof; and further comprises adding reagent selected from a group comprising alkaline metal carbonate and alkaline earth metal carbonate or a combination thereof.3. The process as claimed in claim 2 , wherein volume of the solvent ranges from about 1 to about 30 volumes; and wherein the alkaline metal carbonate and alkaline earth metal carbonate is selected from a group comprising lithium carbonate claim 2 , sodium carbonate claim 2 , potassium carbonate claim 2 , cesium carbonate claim 2 , magnesium carbonate claim 2 , calcium carbonate and barium carbonate.4. The process as claimed in claim 1 , wherein the step (a) is carried out at temperature ranging from about 10° C. to about 160° C. and for a time period ranging from about 3 hours to about 24 hours.5. The process as claimed in claim 1 , wherein the conversion of step (b) or step (c) or step (d) is carried ...

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Номер записи: 50

14-01-2016 дата публикации

PROCESS FOR PREPARING SUBSTITUTED PHENYLALKANES

Номер: US20160009635A1

Автор: Liao Subo, McClurg Joseph, Trawick Bobby

Принадлежит:

The invention provides methods for preparing substituted phenylalkanes. In particular, the processes comprise reacting a phenyl boronic compound with an α-β unsaturated carbonyl-containing compound via an asymmetric 1,4-addition reaction. The processes may be useful in the synthesis of tapentadol. 2. The process of claim 1 , wherein Ris hydrogen claim 1 , alkyl claim 1 , or substituted alkyl; Ris alkyl or substituted alkyl; R claim 1 , R claim 1 , R claim 1 , and Rare independently hydrogen claim 1 , alkyl claim 1 , substituted alkyl claim 1 , hydroxyl claim 1 , alkoxy claim 1 , substituted alkoxy claim 1 , aryl claim 1 , substituted aryl claim 1 , alkylaryl claim 1 , or substituted alkylaryl; Rand Rare independently alkyl or substituted alkyl; and Rand Rare independently hydrogen claim 1 , alkyl claim 1 , aryl claim 1 , or alkylaryl.3. The process of claim 2 , wherein Ris C-Calkyl; Ris C-Calkyl; R claim 2 , R claim 2 , R claim 2 , and Rare hydrogen; and R claim 2 , Rand Rare C-Calkyl.4. The process of claim 1 , wherein R is methyl; Ris hydrogen; Ris ethyl; each of R claim 1 , R claim 1 , R claim 1 , and Ris hydrogen; and R claim 1 , R claim 1 , and Rare methyl.5. The process of claim 1 , wherein the compound of Formula (I) claim 1 , the compound of Formula (VIII) claim 1 , and the transition metal catalyst are present at a molar ratio of about 1:0.5:0.001 to about 1:2.0:0.05; and step (a) is conducted at a temperature from about −10° C. to about 80° C.6. The process of claim 5 , wherein the transition metal catalyst is a transition metal complex chosen from a rhodium complex claim 5 , a palladium complex claim 5 , or a ruthenium complex; the chiral ligand is a bicyclic chiral diene; and the transition metal catalyst and the chiral ligand are present at a weight ratio of about 1:0.1 to about 1:10.7. The process of claim 6 , wherein the compound of Formula (IX) is obtained with a diastereomeric excess of at least about 60%.8. The process of claim 6 , wherein step (a) ...

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Номер записи: 51

27-01-2022 дата публикации

PROCESS FOR MANUFACTURING ETHYLENEAMINE COMPOUNDS

Номер: US20220024852A1

Автор: EDVINSSON Rolf Krister, EHLERS Ina, JOVIC Slavisa, KANTZER Eike Nicolas, LAKE Karl Fredrik, RAAIJMAKERS Michiel Jozef Thomas, TEN KATE Antoon Jacob Berend, VAN DAM Hendrik, VENEMAN Rens, ZUBEIR Lawien Feisal

Принадлежит: NOURYON CHEMICALS INTERNATIONAL B.V.

The present disclosure pertains to a process for manufacturing ethyleneamine compounds selected from the group of ethyleneamines and hydroxyethylethyleneamines wherein the process comprises two reaction sequences. 1. Process for manufacturing ethyleneamine compounds selected from the group of ethyleneamines and hydroxyethylethyleneamines wherein the process comprises a first and a second reaction sequences , in an adduction step, providing a CO2 adduct of a starting compound comprising a —NH—CH2-CH2-NH— moiety or a —NH—CH2-CH2-OH moiety, or HO—CH2-CH2-OH,', 'in a chain-extension step reacting a hydroxy-functional compound selected from ethanolamines and dihydroxyethane with an ethyleneamine compound, wherein at least part of a total of hydroxy-functional compounds and the ethyleneamine compound is provided in the form of a CO2 adduct, to form a CO2 adduct of a chain-extended ethyleneamine compound,', 'in an elimination step converting the CO2 adduct of the chain-extended ethyleneamine compound to the corresponding product ethyleneamine compound by removal of the carbonyl group, and, 'the first reaction sequence comprising the steps of in a ethylenedichloride reaction step reacting ethylenedichloride with at least one compound selected from the group of ammonia, an ethyleneamine and/or an ethanolamine to form a hydrochloride salt of the ethyleneamine and/or the ethanolamine,', 'in a caustic treatment step reacting a hydrochloride salt of the ethyleneamine or ethanolamine with a base to form an ethyleneamine compound and an inorganic chloride salt,', 'in a salt separation step separating the inorganic chloride salt from the ethyleneamine compound,, 'the second reaction sequence comprising the steps of effluent from a step in the first reaction sequence is provided as a starting material to a step in the second reaction sequence,', 'effluent from a step in the second reaction sequence is provided as a starting material to a step in the first reaction sequence,', 'a ...

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Номер записи: 52

14-01-2021 дата публикации

METHODS FOR PRODUCING (6S,15S)-3,8,13,18-TETRAAZAICOSANE-6,15-DIOL

Номер: US20210009504A1

Автор: Bharathkumar Padavalachandu, PATIL Rahul, Rai U Sankappa, Shanker P. Sathya, Vengatesan Selvam, Venghatraghavan Murali

Принадлежит:

The present invention provides methods of synthesizing (6S,15S)-3,8,13,18-tetraazaicosane-6,15-diol and salts thereof. 2. The method of claim 1 , wherein PG is benzyl or substituted benzyl.3. The method of claim 2 , wherein PG is benzyl claim 2 , 4-methoxybenzyl or 3 claim 2 ,4-dimethoxybenzyl.4. The method of claim 3 , wherein PG is benzyl.5. The method of claim 2 , wherein in step (e) claim 2 , the compound of Formula (VI) is deprotected by hydrogenolysis.6. The method of claim 4 , further comprising the step of reacting 1 claim 4 ,4-diaminobutane with benzaldehyde under reducing conditions claim 4 , thereby producing the compound of Formula (I).7. The method of claim 1 , wherein the reducing agent of step (b) is lithium aluminum hydride.8. The method of claim 1 , wherein the acetylating agent is acetic anhydride.9. The method of claim 1 , wherein the reducing agent of step (d) is lithium aluminum hydride.10. The method of claim 1 , wherein PG is benzyl; the reducing agent of step (b) and the reducing agent of step (d) are both lithium aluminum hydride; and the acetylating agent is acetic anhydride.11. The method of claim 1 , wherein step (a) is conducted in the presence of a base.12. The method of claim 11 , wherein the base is KCO claim 11 , NaHCOor diisopropylethylamine.13. The method of claim 11 , where step (a) is conducted in a polar organic solvent.14. The method of claim 13 , wherein the solvent is ethanol claim 13 , N claim 13 ,N-dimethylformamide claim 13 , or acetone.15. The method of claim 1 , wherein step (a) is conducted in an ethanol solution of sodium bicarbonate.16. The method of claim 1 , wherein the reducing agent in step (b) is lithium aluminum hydride or Raney nickel and ammonia.17. The method of claim 1 , wherein step (b) is conducted in tetrahydrofuran or methanolic ammonia. This application is a continuation of International Application No. PCT/US2019/015581, which designated the United States and was filed on Jan. 29, 2019, published in ...

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Номер записи: 53

21-01-2016 дата публикации

NONIONIC SURFACTANT COMPOSITIONS

Номер: US20160016886A1

Автор: Elowe Paul R., Graf Irina V., Krasovskiy Arkady L., WANG Lin

Принадлежит:

The present invention provides nonionic surfactants, compositions incorporating these surfactants, and related methods of making and using such surfactants and compositions. The nonionic surfactants demonstrate excellent equilibrium and dynamic surface tension properties as well as excellent wetting properties. Further, representative embodiments of the surfactants have shown low foaming characteristics, indicating that the surfactants would be suitable in applications where resistance to foaming is desired. The surfactants can be used singly or in combination with other nonionic and/or ionic surfactants as desired. As an over view, the nonionic surfactants of the present invention have a structure in which the surfactant backbone includes one or more amine moieties. At least one, preferably two or more branched, cyclic, fused cyclic, and/or spyro hydrophobic moieties are pendant from at least one of the amine moieties. Additionally, at least one, preferably two or more hydrophilic moieties, preferably alkylene oxide (i.e., polyether) chains also are pendant from at least one of the amine moieties. 1. A method of making a nonionic surfactant , comprising the steps of:a) providing an adduct comprising at least one secondary amine moiety and at least two branched, cyclic, fused cyclic, and/or spyro hydrophobic moieties; andb) N-functionalizing at least a portion of the secondary amine moieties of the adduct under conditions effective to convert at least a portion of the secondary amine moieties to tertiary amine moieties having pendant, hydrophilic, N-ether functionality.2. The method of claim 1 , wherein step (a) comprises reacting ingredients comprising first and second compounds under conditions effective to form the adduct claim 1 , wherein the first compound comprises one or more ketone and/or aldehyde moieties and the second compound comprises one or more primary amine moieties.3. The method of claim 2 , wherein the first compound comprises one or more of methyl ...

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Номер записи: 54

18-01-2018 дата публикации

FLUORINE-CONTAINING ETHER MONOCARBOXYLIC ACID AMINOALKYL ESTER AND A METHOD FOR PRODUCING THE SAME

Номер: US20180016223A1

Автор: KOKIN Keisuke

Принадлежит:

A fluorine-containing ether monocarboxylic acid aminoalkyl ester represented by the general formula: 2. The fluorine-containing ether monocarboxylic acid aminoalkyl ester according to claim 1 , wherein a is an integer of 4 to 10 claim 1 , and b is an integer of 1 to 3.4. The method for producing the fluorine-containing ether monocarboxylic acid aminoalkyl ester according to claim 3 , wherein after completion of the reaction claim 3 , the reaction mixture is treated with an alkali metal hydroxide aqueous solution. The present invention relates to a fluorine-containing ether monocarboxylic acid aminoalkyl ester and a method for producing the same. More particularly, the present invention relates to a fluorine-containing ether monocarboxylic acid aminoalkyl ester that is imparted with flexibility in a molecular chain due to an ether bond in a molecule, and that is effectively used as a synthetic raw material, etc.; and also relates to a method for producing the same.Heretofore, the present applicant has proposed various fluoroethers having a terminal alkylamino group, to which flexibility in the molecular chain is imparted by an ether linkage in the molecule, or fluorine-containing polyether carboxylic acid amides (see Patent Documents 1 to 7). Further, the present applicant has also proposed fluorine-containing acid fluoride compounds having COOH, CONH, or the like at the molecular end (see Patent Document 8).However, there has been hardly observed finding on fluorine-containing ether carboxylic acid esters having an amino group at the end of the ester group.Patent Document 1: WO 2007/026513Patent Document 2: JP-A-2008-255042Patent Document 3: JP-A-2009-1709Patent Document 4: JP-A-2010-254736Patent Document 5: JP-A-2011-202055Patent Document 6: JP-A-2011-213837Patent Document 7: JP-A-2013-32455Patent Document 8: JP-A-2008-255035Patent Document 9: JP-A-3-284642Patent Document 10: JP-A-62-270546An object of the present invention is to provide a fluorine-containing ether ...

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Номер записи: 55

15-01-2015 дата публикации

PROCESS FOR PRODUCING N-METHYL OR N,N-DIMETYL AMINES

Номер: US20150018548A1

Автор: Cui Xinjiang, Deng Youquan, Shi Feng, Yuan Hangkong, Zhang Yan

Принадлежит: Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences

A process for producing N-methyl or N,N-dimethyl amines, which comprises using amine compound, nitro-containing compound or nitrile compound as a starting material, carbon dioxide as a methylating agent and hydrogen gas as a reducing agent, and allowing them to react in a sealed reactor for 6 to 48 h in a reaction medium at a reaction temperature of 80 to 180 ° C. in the presence of a composite catalyst, so as to provide N-methyl or N,N-dimethyl amines. The process of the present invention is simple and under relative mild reaction conditions. By means of the process of the invention, the target products can be prepared at low cost with a high yield. The catalysts used have a high catalytic activity and can be separated from the reaction system simply and reused. Furthermore, the whole process of the present invention is environmental-friendly and facilitates the cycling use of carbon dioxide. 1. A process for producing N-methyl or N ,N-dimethyl amines comprisingusing amine compound, nitro-containing compound or nitrile compound as a starting material, carbon dioxide as a methylating agent, and hydrogen gas as a reducing agent, and allowing them to react in a reaction medium in a sealed reactor for 6 to 48 h at a reaction temperature of 80 to 180° C. in the presence of a composite catalyst, to provide the N-methyl or N,N-dimethyl amines,wherein the composite catalyst is formed of oxides of at least two metals, or of oxide of at least one metal and at least another metal element, said metal or metal element is selected from the group consisting of aluminum, bismuth, zinc, tin, gold, silver, copper, nickel, palladium, platinum, iridium, rhodium, cobalt, iron, ruthenium, osmium, manganese, rhenium, chromium, molybdenum, tungsten, vanadium, titanium, zirconium, lanthanum, yttrium, cerium, magnesium, calcium and barium.2. The process according to claim 1 , wherein the molar ratio of the methylating agent to the starting material is 1:1˜20:1 and the molar ratio of the ...

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Номер записи: 56

16-01-2020 дата публикации

Catalytic Process For Preparing N,N-Dimethylglucamine From N Methylglucamine

Номер: US20200017435A1

Автор: Akgün Ertan, Klug Peter, KREUZPOINTNER Stefan, LINK Martin, RAAB Klaus, SCHEITZENEDER Karl, WERNER Sarah

Принадлежит: CLARIANT INTERNATIONAL LTD.

The invention relates to a method for preparing aqueous solutions of N,N-dimethylglucamine, characterized by first preparing an adduct of N-methylglucamine and formaldehyde in water at temperatures of between 15° C. and 40° C., and subsequently reacting said adduct to N,N-dimethylglucamine in the presence of a metal catalyst under hydrogen pressure at 20-68° C., followed by secondary hydrogenation at 70-120 bar and 70-110° C. once hydrogen absorption at 20-68° C. is completed. 1. A process for preparing N ,N-dimethylglucamine comprising the step of reacting an aqueous solution of N-methylglucamine first with an aqueous solution of formaldehyde at 15-40° C. and subsequently , at a pressure of 20-120 bar and a temperature T=30-68° C. , with hydrogen under metal catalysis , wherein , after absorption of hydrogen has completed at 20-68° C. , a further , after-hydrogenation is added at 70-120 bar and at 70-110° C.2. The process as claimed in claim 1 , wherein the metal catalyst is Raney nickel.3. The process as claimed in claim 1 , which is carried out at a hydrogen pressure of 70-110 bar.4. The process as claimed in claim 1 , wherein the hydrogenation is carried out at 35-65° C.5. The process as claimed in claim 1 , wherein the molar ratio of N-methylglucamine to formaldehyde is 1:1 to 1:1.5.6. The process as claimed in claim 1 , wherein the hydrogenation catalyst is reused more than 5 times.7. The process as claimed in claim 1 , wherein reaction takes place in a stirred reactor or loop reactor.8. The process as claimed in claim 1 , wherein the remaining N-methylglucamine content is <2 claim 1 , wt %.9. The process as claimed in claim 1 , wherein the residual formaldehyde content is <0.1 wt %.10. The process as claimed in claim 1 , in which the Hazen color number of the resulting solution of N claim 1 ,N-dimethylglucamine is <500.11. The process as claimed in claim 1 , in which the molar ratio of N-methylglucamine to formaldehyde is 1:1 to 1:1.2.12. The process as ...

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Номер записи: 57

26-01-2017 дата публикации

MINIMIZING WATER CONTENT IN ETHANOLAMINE PRODUCT STREAMS

Номер: US20170022145A1

Автор: Al-Hazmi Naeem

Принадлежит: Sabic Global Technologies B.V.

Systems and method are provided for reducing the water content in ethanolamine product streams from approximately 0.15%-0.19% by weight of water to approximately 0.02 to approximately 0.04 by weight of water. The reduced water content can be achieved by increasing the processing conditions at the monoethanolamine column by approximately 5% to approximately 20%, more preferably to approximately 10%, and by adding a dummy stream to the monoethanolamine column, which can be recycled to the reactor. The increased processing conditions and dummy stream at the monoethanolamine column can result in the following to achieve said water content: (i) the bottom stream flow rate increase by up to approximately 18.9%; the reboiler duty can be increased by up to 47.9%; and (iii) the condenser duty can be increased by up to approximately 52.5%. 1. A method for producing an ethanolamine product stream in a non-reactive distillation column , comprising:mixing an ammonia solution comprising approximately 30% to approximately 40% by weight ammonia with ethylene oxide in a reactor to create a resultant product stream, wherein said resultant product stream comprises ethanolamines, unreacted ammonia and water;removing approximately 30% to approximately 50% by weight of the unreacted ammonia and approximately 50% to approximately 70% by weight of water from the resultant product stream to create a stripped product stream, wherein the stripped product stream comprises ethanolamines and approximately 30% to approximately 50% by weight of water;transferring the stripped product stream to at least one stage of a vacuum drying column to create a dehydrated product stream;transferring the dehydrated product stream to at least one stage of a monoethanolamine distillation column to create a distilled product stream, wherein the dehydrated product stream comprises ethanolamines and approximately 0.01% to approximately 0.1% by weight of water;operating the monoethanolamine distillation column at ...

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Номер записи: 58

17-04-2014 дата публикации

METHODS FOR PRODUCING EPOXIDATION CATALYSTS AND EPOXIDATION METHODS UTILIZING THEM

Номер: US20140107356A1

Автор: Basrur Arun G., Gopal Srikant, Murthy Lakshmi N. Vutukuru

Принадлежит: DOW TECHNOLOGY INVESTMENTS, LLC

A method for producing epoxidation catalysts is provided. The catalyst comprises a support, a catalytic species, maganese and at least one alkali metal and/or promoter. The catalytic species may be silver. The catalyst is prepared by a method wherein at least a portion of the manganese is impregnated in a step separate from the at least one alkali metal and/or promoter. Advantageously, catalysts produced by the present method may exhibit greater efficiencies than catalysts produced by conventional methods. A method for the epoxidation of alkylenes using the catalysts so produced is provided as is a method for using the alkylene oxides for the production of 1,2-diols, 1,2-carbonates, 1,2-diol ethers, or alka-nolamines. 1. A method for making an epoxidation catalyst comprising a support , at least one catalytic species , manganese and at least one alkali metal and/or promoter , comprising:Impregnating at least a portion of the manganese in an impregnation step separate from the at least one alkali metal and/or promoter.2. The method of claim 1 , wherein the manganese is impregnated with the at least one catalytic species.3. The method of claim 1 , wherein the at least one alkali metal and/or promoter comprises sodium claim 1 , cesium claim 1 , lithium claim 1 , sulfate or combinations of these.4. The method of claim 1 , wherein the at least one alkali metal and/or promoter comprises sodium and is impregnated in a step separate from the manganese.5. The method of claim 1 , wherein the manganese comprises Mn-EDTA complex.6. The method of claim 1 , wherein the at least one alkali metal and/or promoter comprises rhenium.7. The method of claim 1 , wherein the catalytic species comprises silver.8. An epoxidation catalyst prepared according to the method of .9. A method for the epoxidation of one or more alkylenes comprising contacting an oxygen source and an alkylene in the presence of an epoxidation catalyst prepared according to the method of .10. The method of claim 8 , ...

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Номер записи: 59

25-01-2018 дата публикации

METHOD FOR PRODUCING 2-AMINOETHYLMETHACRYLATE HYDROCHLORIDE

Номер: US20180022692A1

Автор: IIDA Yuri, Sato Hideyuki, TAKEMOTO Masaki

Принадлежит: MITSUBISHI GAS CHEMICAL COMPANY, INC.

Provided is a method for producing 2-aminoethyl methacrylate hydrochloride that, according to one embodiment, includes a step (A) for reacting a ketimine compound of 2-aminoethyl methacrylate with water and hydrogen chloride and obtaining a mixture containing 2-aminoethyl methacrylate hydrochloride, wherein in the step (A), the ratio of the total amount of hydrogen chloride to the total amount of ketimine compound of 2-aminoethyl methacrylate is 1.0-1.5 expressed in terms of equivalents, and the ratio of the total amount of water to the total amount of ketimine compound of 2-aminoethyl methacrylate is 1.0-2.0 expressed in terms of equivalents. 2. The method for producing 2-aminoethyl methacrylate hydrochloride according to claim 1 , wherein Rand Rin Formula (1) above each independently represent an alkyl group with a carbon number of 1-4.3. The method for producing 2-aminoethyl methacrylate hydrochloride according to claim 2 , wherein claim 2 , in Formula (1) above claim 2 , Rrepresents a methyl group and Rrepresents an ethyl group or an isobutyl group.4. The method for producing 2-aminoethyl methacrylate hydrochloride according to claim 3 , wherein Rin Formula (1) above represents an isobutyl group.5. The method for producing 2-aminoethyl methacrylate hydrochloride according to claim 3 , wherein Rin Formula (1) above represents an ethyl group.6. The method for producing 2-aminoethyl methacrylate hydrochloride according to claim 1 , wherein hydrogen chloride is hydrogen chloride gas.7. The method for producing 2-aminoethyl methacrylate hydrochloride according to claim 1 , wherein the reaction of the ketimine compound of 2-aminoethyl methacrylate represented by Formula (1) with water and hydrogen chloride is carried out such that the ratio of the accumulated supply amount of hydrogen chloride to the accumulated supply amount of the ketimine compound of 2-aminoethyl methacrylate is maintained at 1.0 or higher in equivalent ratio throughout the whole period from the ...

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Номер записи: 60

25-01-2018 дата публикации

1, 1' -BIS(PHOSPHINO)FERROCENE LIGANDS FOR ALKOXYCARBONYLATION

Номер: US20180022773A1

Автор: Beller Matthias, DONG Kaiwu, DYBALLA Katrin Marie, Franke Robert, Fridag Dirk, GEILEN Frank, HESS Dieter, Jackstell Ralf, NEUMANN Helfried

Принадлежит: EVONIK DEGUSSA GmbH

Compound of formula (I) 2. Compound according to claim 1 ,{'sup': 2', '4, 'sub': 1', '12, 'where R, Rare each independently selected from —(C-C)-alkyl, cyclohexyl and phenyl.'}3. Compound according to claim 1 ,{'sup': 1', '3, 'where the R, Rare each a heteroaryl radical having five to ten ring atoms.'}4. Compound according to claim 1 ,{'sup': 1', '3, 'where R, Rare each independently selected from furyl, thienyl, pyrrolyl, oxazolyl, isoxazolyl, thiazolyl, isothiazolyl, imidazolyl, pyrazolyl, furazanyl, tetrazolyl, pyridyl, pyridazinyl, pyrimidyl, pyrazinyl, benzofuranyl, indolyl, isoindolyl, benzimidazolyl, quinolyl, isoquinolyl.'}5. Compound according to claim 1 ,{'sup': 1', '3, 'where Rand Rare each pyridyl.'}6. Compound according to claim 1 ,{'sup': 1', '3', '2', '4, 'where Rand Rare each identical radicals and Rand Rare each identical radicals.'}8. Complex comprising Pd and a compound according to .9. Process comprising the following process steps:a) initially charging an ethylenically unsaturated compound;{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, 'b) adding a compound according to and a compound comprising Pd;'}c) adding an alcohol;d) feeding in CO;e) heating the reaction mixture, with conversion of the ethylenically unsaturated compound to an ester.10. Process according to claim 9 ,wherein the ethylenically unsaturated compound comprises 2 to 30 carbon atoms and optionally one or more functional groups selected from carboxyl, thiocarboxyl, sulpho, sulphinyl, carboxylic anhydride, imide, carboxylic ester, sulphonic ester, carbamoyl, sulphamoyl, cyano, carbonyl, carbonothioyl, hydroxyl, sulphhydryl, amino, ether, thioether, aryl, heteroaryl or silyl groups and/or halogen substituents.11. Process according to claim 9 ,wherein the ethylenically unsaturated compound is selected from ethene, propene, 1-butene, cis- and/or trans-2-butene, isobutene, 1,3-butadiene, 1-pentene, cis- and/or trans-2-pentene, 2-methyl-1-butene, 3-methyl-1-butene, 2-methyl-2-butene, ...

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Номер записи: 61

02-02-2017 дата публикации

AMINE FOR LOW-EMISSION EPOXY RESIN PRODUCTS

Номер: US20170029364A1

Автор: BURCKHARDT Urs, KASEMI Edis, KRAMER Andreas, STADELMANN Ursula

Принадлежит: SIKA TECHNOLOGY AG

The present invention relates to an amine of the formula (I) which is an adduct of 1,2-propylenediamine with an aryl monoglycidyl ether, to the use thereof as part of a hardener for epoxy resins, and to epoxy resin compositions obtained therewith. The amine of the formula (I) is preparable in a simple process in high purity, is of very low viscosity and is especially suitable for the curing of epoxy resins. It allows low-emission epoxy resin compositions which have good workability and which cure even under cold and damp conditions, quickly and without blushing effects, to form very hard products of high surface quality that display virtually no yellowing on exposure to light. 2. The amine as claimed in claim 1 , wherein n is 1.3. The amine as claimed in claim 1 , wherein R is methyl.4. A process for preparing an amine as claimed in by reacting 1 claim 1 ,2-propylenediamine with an aryl glycidyl ether in a 1 claim 1 ,2-propylenediamine/aryl glycidyl ether molar ratio in the range from 1.1 to 5 and subsequent distillative removal of unreacted 1 claim 1 ,2-propylenediamine.5. A method wherein at least one amine as claimed in is used in a hardener for epoxy resins.6. The method as claimed in claim 5 , wherein the hardener comprises an amine of formula (I) in an amount such that 5 to 100% of the amine hydrogens in the hardener that are reactive toward epoxide groups originate from the amine of the formula (I).7. The method as claimed in claim 5 , wherein the hardener as well as the amine of the formula (I) comprises at least one further polyamine having at least two amine hydrogens that are active toward epoxide groups.8. The method as claimed in claim 7 , wherein the further polyamine is a primary diamine selected from the group consisting of 2 claim 7 ,2 claim 7 ,4- and 2 claim 7 ,4 claim 7 ,4-trimethylhexamethylenediamine claim 7 , 1-amino-3-aminomethyl-3 claim 7 ,5 claim 7 ,5-trimethylcyclohexane claim 7 , 1 claim 7 ,3-bis(aminomethyl)benzene claim 7 , 1 claim 7 ,3- ...

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Номер записи: 62

04-02-2016 дата публикации

ANTIMUSCARINIC COMPOUND HAVING A LOW CONTENT OF IMPURITIES

Номер: US20160031796A1

Автор: Allegrini Pietro, Attolino Emanuele, GRAZIOSI Renzo

Принадлежит: DIPHARMA FRANCIS S.R.L.

Substantially stable to degradation Fesoterodine fumarate, a process for its preparation and a process for the synthesis of specific degradation impurities of Fesoterodine fumarate are disclosed. 1. A process for the preparation of a substantially stable to degradation Fesoterodine fumarate , comprising:the salification of Fesoterodine base with fumaric acid in the presence of a solvent wherein the molar ratio between Fesoterodine base and fumaric acid is comprised between about 1:0.10 and about 1:0.88;the precipitation of Fesoterodine fumarate from the resulting solution;the recovery of the solid.2. Process according to wherein the Fesoterodine base to fumaric acid molar ratio is comprised between about 1:0.5 and about 1:0.85.4. Process according to wherein the molar ratio of the compound of formula (IV) to fumaric acid is comprised between about 1:0.4 and about 1:0.80.6. A substantially stable to degradation Fesoterodine fumarate as obtainable according to the process of .7. Fesoterodine fumarate according to claim 5 , having a total content of the impurities of formula (VI) claim 5 , (VII) (VIII) or (IX) equal to or lower than 0.1% claim 5 , and preferably comprised between about 0.1% and about 0.01% claim 5 , calculated as Area % by HPLC.8. A pharmaceutical composition comprising substantially stable to degradation Fesoterodine fumarate according to and a pharmaceutically acceptable carrier and/or excipient.9. A substantially stable to degradation Fesoterodine fumarate claim 5 , according to claim 5 , for use as a medicament claim 5 , in particular in a method of treatment of urinary incontinence in a mammal in need thereof. The invention relates to a process for the preparation of (R)-2-(3-diisopropylamino-1-phenylpropyl)-4-(hydroxymethyl)phenol isobutyrate (Fesoterodine) as fumarate salt, substantially stable as herein defined, that is Fesoterodine fumarate which substantially does not develop degradation impurities; and a method for the preparation of ...

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Номер записи: 63

29-01-2015 дата публикации

PROCESS FOR THE PRODUCTION OF CHOLINE HYDROXIDE

Номер: US20150031917A1

Автор: Moonen Kristof, SCHELDEMAN Daan, Ulrichts Dieter

Принадлежит: TAMINCO

A continuous process for the production of choline hydroxide includes reacting ethylene oxide, trimethylamine, and water in a reaction zone to form a reaction mixture and extracting heat from the reaction mixture. Subsequently, phase separation of the s reaction mixture is induced to obtain a choline hydroxide phase and an organic liquid phase comprising trimethylamine. A choline hydroxide solution (e.g., at a concentration of about 40% to 50% by weight, based on total weight of the choline hydroxide solution) is obtained from the choline hydroxide phase. 1. A continuous process for the production of choline hydroxide comprising:reacting ethylene oxide, trimethylamine, and water in a reaction zone to form a reaction mixture;extracting heat from the reaction mixture;subsequently, inducing phase separation of the reaction mixture to obtain a choline hydroxide phase and an organic liquid phase comprising trimethylamine; andobtaining a choline hydroxide solution from the choline hydroxide phase.2. The process according to claim 1 , wherein the reaction zone comprises an excess of the trimethylamine as a reaction medium.3. The process according to claim 1 , wherein the choline hydroxide solution is subsequently treated to remove residual trimethylamine or O-ethoxylated side products.4. The process according to claim 1 , wherein the organic liquid phase comprises less than 5% by weight of choline hydroxide.5. The process according to claim 1 , wherein the heat is extracted by passing the reaction mixture through a heat exchanger.6. The process according to claim 1 , wherein the phase separation occurs in a decanter.7. The process according to claim 1 , wherein the phase separation provides a top layer comprising liquid trimethylamine and a bottom layer comprising choline hydroxide and water.8. The process according to claim 1 , wherein the organic liquid phase is recycled to an inlet of the reaction zone.9. The process according to claim 1 , wherein the choline hydroxide ...

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Номер записи: 64

01-02-2018 дата публикации

Method for preparing 4-isopropylamino-1-butanol

Номер: US20180029973A1

Автор: Chi Ma, Fanghui TANG, Qiang JIA

Принадлежит: Seasons Biotechnology (taizhou) Co Ltd

The present invention relates to a preparation method of 4-isopropylamino-1-butanol, in which using cheap and readily available tetrahydrofuran and acetic acid solution of hydrogen bromide as starting materials to prepare a novel intermediate of 4-isopropylamino-1-acetoxyl butane and further obtain the target product. The present invention has advantages of convenient process operations, mild reaction conditions, economical and environment-friendly benefits, and suitability for industrial production to obtain the product with high purity and high yield.

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Номер записи: 65

01-02-2018 дата публикации

COMPOSITION CONTAINING 3-CHLORO-4-METHOXYBENZYLAMINE HYDROCHLORIDE, AND METHOD FOR PRODUCING SAME

Номер: US20180029974A1

Автор: FUJIMOTO Takashi, IDE Takahiro, YOKOTA Keiichi

Принадлежит:

There is provided a method for producing, at a high yield, a composition containing 3-chloro-4-methoxybenzylamine hydrochloride (CMBA-HCl) in which the purity of CMBA-HCl is high. This method comprises a chlorination step involving a chlorination reaction that generates CMBA-HCl from 4-methoxybenzylamine hydrochloride using hydrogen peroxide and hydrochloric acid. There is also provided a CMBA-HCl-containing composition which is produced by the aforementioned production method and in which the purity of CMBA-HCl is high. 1. A method for producing a composition containing 3-chloro-4-methoxybenzylamine hydrochloride , the method comprising a chlorination step involving a chlorination reaction that generates 3-chloro-4-methoxybenzylamine hydrochloride from 4-methoxybenzylamine hydrochloride using hydrogen peroxide and hydrochloric acid.2. A method for producing a composition containing 3-chloro-4-methoxybenzylamine hydrochloride , the method comprising a purification step of recrystallizing a composition containing 3-chloro-4-methoxybenzylamine hydrochloride using a solvent containing a tertiary amine.3. A method for producing a composition containing 3-chloro-4-methoxybenzylamine hydrochloride , the method comprising:a chlorination step involving a chlorination reaction that generates 3-chloro-4-methoxybenzylamine hydrochloride from 4-methoxybenzylamine hydrochloride using hydrogen peroxide and hydrochloric acid; anda purification step of recrystallizing a generated product obtained by the chlorination step, using a solvent containing a tertiary amine.4. The method for producing as recited in claim 1 , wherein a starting material for the chlorination reaction is a composition containing 4-methoxybenzylamine hydrochloride and a content of the 4-methoxybenzylamine hydrochloride is 99.5% or more as a content based on a peak area ratio obtained by HPLC measurement.5. The method for producing as recited in claim 2 , wherein the purification step includes reducing a content ...

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Номер записи: 66

01-02-2018 дата публикации

MANUFACTURING METHOD FOR COMPOUND HAVING N,N-BIS(2-HYROXY-3-CHLOROPROPYL)AMINO GROUP

Номер: US20180030013A1

Автор: Nakatani Jiro, Takezawa Ryota

Принадлежит:

A method efficiently and safely manufactures, on an industrial scale, a compound having an N,N-bis(2-hydroxy-3-chloropropyl)amino group. (1) an amine compound or a solution thereof, (2) epichlorohydrin or a solution thereof, and (3) an acidic compound or a solution thereof are continuously supplied to a flow reactor and reacted at a reaction temperature of 40 to 130° C. and a liquid space velocity of 0.2 to 10 hso that a compound having an N,N-bis(2-hydroxy-3-chloropropyl)amino group is manufactured. The obtained compound having an N,N-bis(2-hydroxy-3-chloropropyl)amino group is dehydrochlorinated by reaction with an alkali so that a polyfunctional glycidylamine type epoxy compound is manufactured. 16-. (canceled)7. A method of manufacturing a compound having an N ,N-bis(2-hydroxy-3-chloropropyl)amino group in which (1) an amine compound or a solution thereof , (2) epichlorohydrin or a solution thereof , and (3) an acidic compound or a solution thereof are continuously supplied to a flow reactor and reacted at a reaction temperature of 40 to 130° C. and a liquid space velocity of 0.2 to 10 h.8. The method according to claim 7 , wherein a tubular reactor is used as the flow reactor.9. The method according to claim 8 , wherein the tubular reactor is charged with a filler.10. The method according to claim 7 , wherein the acidic compound is a Lewis acid or an organic acid.11. The method according to claim 7 , wherein claim 7 , as the amine compound claim 7 , one selected from the group consisting of aniline claim 7 , toluidine claim 7 , phenoxy aniline claim 7 , amino phenol claim 7 , diaminodiphenyl ether claim 7 , diaminodiphenyl methane claim 7 , and diaminodiphenyl sulphone is used.12. A method of manufacturing a polyfunctional glycidylamine type epoxy compound comprising producing the compound having an N claim 7 ,N-bis(2-hydroxy-3-chloropropyl)amino group manufactured according to and dehydrochlorinating the obtained compound having the N claim 7 ,N-bis(2-hydroxy- ...

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Номер записи: 67

05-02-2015 дата публикации

METHODS FOR THE PREPARATION OF HIV ATTACHMENT INHIBITOR PIPERAZINE PRODRUG COMPOUND

Номер: US20150038710A1

Автор: Bultman Michael S., CHEN KE, Eastgate Martin D., Fanfair Dayne Dustan, Fox Richard J., La Cruz Thomas E., Mudryk Boguslaw M., Risatti Christina Ann, Simpson James H., Soumeillant Maxime C., Tripp Jonathan Clive, Xiao Yi

Принадлежит:

A method for making the compound 2. The process of claim 1 , wherein said first solvent is selected from the group of NMP claim 1 , DMSO claim 1 , MeCN claim 1 , MeOH claim 1 , acetone and a carboxylic acid.3. The process of claim 1 , wherein said second solvent is selected from the group of an alkyl ketone claim 1 , heptane claim 1 , toluene claim 1 , and ethyl acetate.4. The process of claim 1 , wherein the first solvent is acetic acid claim 1 , and said second solvent is acetone. This application is a divisional application of U.S. Ser. No. 13/760,526 filed Feb. 6, 2013, now allowed, which claims the benefit of U.S. Provisional Application Ser. No. 61/596,362 filed Feb. 8, 2012, which is herein incorporated by reference in its entirety.The invention relates to methods of making HIV attachment inhibitor compounds useful as antivirals, and in particular, to methods of making the piperazine prodrug compound identified as 1-benzoyl-4-[2-[4-methoxy-7-(3-methyl-1H-1,2,4-triazol-1-yl)-1-[(phosphonooxy)methyl]-1H-pyrrolo[2,3-c]pyridin-3-yl]-1,2-dioxoethyl]-piperazine. The invention also relates to the compounds, including intermediates, obtained by the processes herein set forth.HIV-1 (human immunodeficiency virus-1) infection remains a major medical problem, with tens of millions of people still infected worldwide at the end of 2011. The number of cases of HIV and AIDS (acquired immunodeficiency syndrome) has risen rapidly. In 2005, for example, approximately 5.0 million new infections were reported, and 3.1 million people died from AIDS. Currently available drugs for the treatment of HIV include nucleoside reverse transcriptase (RT) inhibitors or approved single pill combinations: zidovudine (or AZT or RETROVIR®), didanosine (or VIDEX®), stavudine (or ZERIT®) lamivudine (or 3TC or EPIVIR®), zalcitabine (or DDC or HIVID®), abacavir succinate (or ZIAGEN®), Tenofovir disoproxil fumarate salt (or VIREAD®), emtricitabine (or FTC or EMTRIVA®), COMBIVIR® (contains −3TC plus ...

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Номер записи: 68

07-02-2019 дата публикации

PROCESS FOR PRODUCING ALKANOLAMINE

Номер: US20190039997A1

Автор: Ichikawa Daisuke, SUGIYA Takahiro

Принадлежит:

The present invention provides a method of producing an ethanolamine, with a low production ratio of a dialkanolamine (for example, less than 30% by weight). A process for producing an alkanolamine of the present invention includes reacting an alkylene oxide with ammonia to obtain a reaction product containing a monoalkanolamine, a dialkanolamine, and a trialkanolamine; separating the dialkanolamine from the reaction product; and recycling at least a portion of the dialkanolamine for the reaction of an alkylene oxide with ammonia, wherein in the recycling step, the dialkanolamine is supplied in a molar ratio of the alkylene oxide (moles) to a total amount (moles) of ammonia and the dialkanolamine of 0.08 or more and less than 0.26. 1. A process for producing an alkanolamine , the process comprising reacting an alkylene oxide with ammonia to obtain a reaction product containing a monoalkanolamine , a dialkanolamine , and a trialkanolamine; separating the dialkanolamine from the reaction product; and recycling at least a portion of the dialkanolamine for the reaction of an alkylene oxide with ammonia ,wherein in the recycling step, the dialkanolamine is supplied in a molar ratio of the alkylene oxide (moles) to a total amount (moles) of ammonia and the dialkanolamine of 0.08 or more and less than 0.26.2. The process according to claim 1 , wherein in the recycling step claim 1 , the dialkanolamine is supplied in a ratio (weight ratio) of the dialkanolamine to the ammonia of 0.05 or more and less than 0.18.3. The process according to claim 1 , further comprising separating the trialkanolamine from the reaction product claim 1 , wherein a trialkanolamine 1 alkylene oxide adduct is contained in the trialkanolamine isolate in an amount of 0.6% by weight or less.4. The process according to claim 1 , wherein a production ratio of the dialkanolamine is less than 30% by weight. The present invention relates to a method for producing an alkanolamine.As a commercial way of ...

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Номер записи: 69

12-02-2015 дата публикации

Asymmetric Diamine Compounds Containing Two Functional Groups and Polymers Therefrom

Номер: US20150045481A1

Автор: Chung Im Sik, Kim Sang Youl, Kim Sun Dal

Принадлежит:

The present invention relates to a novel diamine compound, wherein two substituents R and R′ are introduced asymmetrically, and a polymer thereof. The polymer may have excellent solubility in the organic solvent and allows for easy processibility after imidization, thus giving proper film maintaining superior properties, such as thermal, mechanical, and optical properties for applications in electrical, electronic, or optical materials. 2: The asymmetrical diamine compound according to claim 1 , wherein R and R′ are hydrocarbyl group comprising fluorine.1: The asymmetrical diamine compound according to claim 1 , wherein L is any one selected from the group consisting of a direct bond claim 1 , —O— claim 1 , and —S—.6: The process for producing the asymmetrical diamine compound according to claim 5 , wherein R and R′ are hydrocarbyl group comprising fluorine.7: The process for producing the asymmetrical diamine compound according to wherein L is any one selected from the group consisting of a direct bond claim 5 , —O— claim 5 , and —S—.9: A process for producing polymer selected from a group of polyamide claim 1 , polyamic acid claim 1 , and polyimide claim 1 , wherein asymmetric diamine compound according to is used in the polymerization as monomer.11: The A process for producing the polyimide according to claim 10 , wherein said asymmetrical diamine compound and tetracarboxylic acid monomers are dissolved in organic solvent to produce polyamic acid claim 10 , followed by heating and stirring to complete imidization.12: The process for producing the polyimide according to claim 10 , wherein said tetracarboxylic acid is any one selected from a group consisting of 1 claim 10 ,2 claim 10 ,4 claim 10 ,5-Benzenetetracarboxylic dianhydride claim 10 , 3 claim 10 ,3′ claim 10 ,4 claim 10 ,4′-Benzophenonetetracarboxylic dianhydride claim 10 , 2 claim 10 ,2′ claim 10 ,3 claim 10 ,3′-Benzophenonetetracarboxylic dianhydride claim 10 , 3 claim 10 ,3′ claim 10 ,4 claim 10 ,4′- ...

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Номер записи: 70

01-05-2014 дата публикации

Process and Apparatus For Production And Filtration Of Aminoalcohols Using A Continuous Stirred Tank Slurry Reactor

Номер: US20140121413A1

Автор: Gummere John D., Major Michael D.

Принадлежит:

Disclosed are processes and apparatuses for producing a reaction product and enabling the reaction product to be removed from a reactor operating at an elevated pressure, while simultaneously maintaining the gas pressure and retaining the catalyst inside the apparatus. 1. An apparatus comprising:a reactor for reacting a first reactant with a second reactant over a catalyst to produce a reaction product;a filtration apparatus for filtering the catalyst from the reaction product, such that the catalyst accumulates in the filtration apparatus; anda backpulse system for returning accumulated catalyst from the filtration apparatus to the reactor.2. An apparatus according to claim 1 , wherein the first reactant and the second reactant are introduced into the filtration apparatus.3. An apparatus according to claim 1 , wherein the backpulse system comprises a first vessel and a second vessel.4. An apparatus according to claim 3 , wherein the first vessel is attached to an outlet of the filtration apparatus.5. An apparatus according to claim 3 , wherein the pressure in the first vessel is greater than the pressure in the reactor.6. An apparatus according to claim 1 , wherein the reactor is a stirred tank slurry reactor.7. An apparatus according to claim 1 , wherein the reactor comprises a plurality of coils to facilitate heat transfer and an agitator to facilitate mass and heat transfer.8. An apparatus according to claim 1 , further comprising a heat exchanger.9. A process comprising:reacting a first reactant with a second reactant over a catalyst in a reactor to produce a reaction product;filtering the reaction product and the catalyst through a filtration apparatus, such that the catalyst accumulates in the filtration apparatus; andreturning accumulated catalyst from the filtration apparatus to the reactor using at least one backwards pulse from a backpulse system.10. A process according to claim 9 , wherein the backpulse system comprises a first vessel and a second vessel ...

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Номер записи: 71

01-05-2014 дата публикации

Process for Preparing Primary Intermediates for Dyeing Keratin Fibers

Номер: US20140121415A1

Автор: GARDLIK John Michael, GARRETT Garry Steven, Murphy Bryan Patrick, Patten Monica Jo

Принадлежит: The Procter & Gamble Company

A process has been developed for preparing 2-methoxymethyl-1,4-benzenediamine (IV-a), other compounds of formula (IV), and the salts thereof, all of which may be used as primary intermediates in compositions for dyeing keratin fibers. 3. The process according to claim 1 , wherein the carbonyl reduction of the compound of formula (I) into the compound of formula (II) is performed in the presence of a carbonyl reducing agent claim 1 , a carbonyl reduction catalyst claim 1 , and a solvent.4. The process according to claim 3 , wherein the carbonyl reducing agent is selected from the group consisting of hydrazine claim 3 , hydrazine hydrate claim 3 , H claim 3 , LiAlH claim 3 , LiBH claim 3 , DIBAL-H claim 3 , NaBH claim 3 , NaCNBH claim 3 , BH claim 3 , BH/THF claim 3 , sodium hydrosulfite claim 3 , sodium sulfide claim 3 , and mixtures of thereof.5. The process according to claim 3 , wherein the carbonyl reduction catalyst is selected from the group consisting of Raney nickel claim 3 , nickel claim 3 , palladium claim 3 , Lindlar' s catalyst claim 3 , cobalt claim 3 , copper chromite claim 3 , platinium claim 3 , platinum oxide claim 3 , rhenium claim 3 , tin(II) chloride claim 3 , titanium(III) chloride claim 3 , zinc claim 3 , samarium claim 3 , iron and mixtures thereof.6. The process according to claim 1 , wherein the etherification of the compound of formula (II) into the compound of formula (III) is performed by alkylation in the presence of an alkylating agent claim 1 , a phase transfer catalyst claim 1 , a solvent claim 1 , and a base.7. The process according to claim 6 , wherein the alkylating agent is selected from the group consisting of methanol claim 6 , (C-C)—I claim 6 , (C-C)—Br claim 6 , (C-C)—Cl claim 6 , MeSO claim 6 , and mixtures thereof.8. The process according to claim 6 , wherein the phase transfer catalyst is selected from the group consisting of ammonium salts that include tetrapentylammonium bromide claim 6 , tetraoctylammonium chloride claim ...

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Номер записи: 72

16-02-2017 дата публикации

Composition containing 3-chloro-4-methoxybenzylamine hydrochloride, and method for producing same

Номер: US20170044091A1

Автор: Keiichi Yokota, Takahiro Ide, Takashi Fujimoto

Принадлежит: AIR WATER INC

There is provided a method for producing, at a high yield, a composition containing 3-chloro-4-methoxybenzylamine hydrochloride (CMBA-HCl) in which the purity of CMBA-HCl is high. This method comprises a chlorination step involving a chlorination reaction that generates CMBA-HCl from 4-methoxybenzylamine hydrochloride using hydrogen peroxide and hydrochloric acid. There is also provided a CMBA-HCl-containing composition which is produced by the aforementioned production method and in which the purity of CMBA-HCl is high.

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Номер записи: 73

15-02-2018 дата публикации

SYSTEMS AND METHODS RELATED TO THE PRODUCTION OF ETHYLENE OXIDE, ETHYLENE GLYCOL, AND/OR ETHANOLAMINES

Номер: US20180044308A1

Автор: Ahmed Labeeb Chaudhary, Al-Hammad Ali, Al-Jaloud Abdullah Turki, Al-Khudeer Saud, Al-Qahtani Thabet, Al-Shammari Talal, Bashir Mubarik Ali, Karim Khalid, Khurram Shehzada, Nawaz Zeeshan

Принадлежит:

Disclosed herein is a method comprising the steps of: a) producing a hydrocarbon stream from syngas via a Fischer-Tropsch reaction, wherein the hydrocarbon stream comprises a first C2 hydrocarbon stream comprising ethane and a first ethylene product; b) separating at least a portion of the first C2 hydrocarbon stream from the hydrocarbon stream; c) separating at least a portion of the first ethylene product from the first C2 hydrocarbon stream, thereby producing a second C2 hydrocarbon stream; d) converting at least a portion of the ethane in the second C2 hydrocarbon stream to a second ethylene product; and e) producing ethylene oxide from at least a portion of the second ethylene product. 1. A method comprising the steps of:producing a hydrocarbon stream from syngas via a Fischer-Tropsch reaction, wherein the hydrocarbon stream comprises a first C2 hydrocarbon stream comprising ethane and a first ethylene product;separating at least a portion of the first C2 hydrocarbon stream from the hydrocarbon stream;separating at least a portion of the first ethylene product from the first C2 hydrocarbon stream, thereby producing a second C2 hydrocarbon stream;converting at least a portion of the ethane in the second C2 hydrocarbon stream to a second ethylene product; andproducing ethylene oxide from at least a portion of the second ethylene product.2. The method of claim 1 , wherein the first C2 hydrocarbon stream comprises from about 30 wt % to about 70 wt % of ethane and from about 70 wt % to about 30 wt % of the first ethylene product.3. The method of wherein the second C2 hydrocarbon stream comprises at least about 80 wt % of ethane.4. The method of claim 1 , wherein the hydrocarbon stream further comprises from about 30 wt % to about 70 wt % of C3-C10 hydrocarbons.5. The method of claim 1 , wherein the method further comprises the step of producing ethylene glycol from at least a portion of the ethylene oxide.6. The method of claim 1 , wherein the method further ...

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Номер записи: 74

03-03-2022 дата публикации

PROCESS FOR PREPARATION OF HIGHLY PURE FINGOLIMOD HYDROCHLORIDE

Номер: US20220064102A1

Автор: CHATURVEDI AKSHAY KANT, Shrawat Vimal Kumar, SINGH SAHDEV

Принадлежит: SHIVALIK RASAYAN LIMITED

The present invention provides process for preparation of highly pure Fingolimod hydrochloride (I),

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Номер записи: 75

25-02-2016 дата публикации

POLYETHERAMINES BASED ON 1,3-DIALCOHOLS

Номер: US20160052867A1

Автор: Boeckh Dieter, CHARRAK Monika, CHRISTMAS Kevin, Ebert Sophia, EICHSTADT WAUN Amy, Eidamshaus Christian, Huelskoetter Frank, LOUGHNANE Brian J., LUDOLPH Bjorn, MAAS Steffen, PANCHENKO Alexander, REES Darren, SCIALLA Stefano, WIGBERS Christof W.

Принадлежит:

This invention relates to polyetheramines based on 1,3-dialcohols, in particular to an etheramine mixture comprising at least 90% by weight, based on the total weight of the etheramine mixture, of anamine of Formula (I) and/or (II), wherein R-Rare independently selected from H, alkyl, cycloalkyl, aryl, alkylaryl, or arylalkyl, wherein at least one of R-Rand at least one of R-Ris different from H, wherein A-Aare independently selected from linear or branched alkylenes having 2 to 18 carbon atoms, preferably 2-10 carbon atoms, most preferably 2-5 carbon atoms, wherein Z-Zare independently selected from OH or NH, wherein at least one of Z-Zand at least one of Z-Zis NH, and wherein the sum of x+y is in the range of from 2 to 200, wherein x≧1 and y≧1; and x+yis in the range of from 2 to 200, preferably 2-20, most preferably 2-10, wherein x≧1 and y≧1. 123.-. (canceled)25. The etheramine mixture according to claim 24 , wherein the etheramine mixture comprises at least 95% by weight claim 24 , based on the total weight of the etheramine mixture claim 24 , of the amine of Formula (I) and/or (II).26. The etheramine mixture according to claim 24 , wherein in said polyetheramine of Formula (I) or Formula (II) claim 24 , x+y is in the range of from 2 to 20.27. The etheramine mixture according to claim 24 , wherein in said polyetheramine of Formula (I) or Formula (II) claim 24 , x+y is in the range of from 3 to 20.28. The etheramine mixture according to claim 24 , wherein in said polyetheramine of Formula (I) or Formula (II) claim 24 , the degree of amination is in the range of 60% to 100%.29. The etheramine mixture according to claim 24 , wherein in said polyetheramine of Formula (I) or Formula (II) claim 24 , A-Aare independently selected from the group consisting of ethylene claim 24 , propylene claim 24 , and butylene.30. The etheramine mixture according to claim 24 , wherein in said polyetheramine of Formula (I) or Formula (II) claim 24 , each of A-Ais propylene.31. The ...

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Номер записи: 76

25-02-2016 дата публикации

Novel Intermediate Used for Preparing Tapentadol or Analogues Thereof

Номер: US20160052873A1

Автор: LI DEGANG, LI XIAOXIANG, XU ZIAO, ZHAO YUANHAI

Принадлежит:

The invention discloses a novel intermediate for preparing tapentadol and analogues thereof, wherein the structural formula is shown as formula I or II, and the groups are defined as the specification. The invention further discloses a method for preparing the novel intermediate and use of the intermediate for preparing tapentadol and analogues thereof. The invention can remarkably improve the product yield and quality of tapentadol, reduce the production cost, and simplify the production procedure. The preparation process is environment friendly, thus more suitable for the requirements of industrial production. 2. The compound according to claim 1 , wherein Ris selected from F claim 1 , Cl claim 1 , Br claim 1 , CHF claim 1 , CF claim 1 , OH claim 1 , SOCH claim 1 , NH claim 1 , CN claim 1 , CHO claim 1 , —Calkyl claim 1 , —Calkoxyl claim 1 , —Ccycloalkyl claim 1 , —Calkylenephenyl claim 1 , —Calkylenenaphthyl claim 1 , tetrahydrofuran or —C(═O)Calkyl; and preferably selected from Cl claim 1 , methyl claim 1 , OH claim 1 , NHor methoxy.3. The compound according to claim 1 , wherein the compound is selected from the following compounds:2-methyl-3-(3-hydroxyphenyl)pentanenitrile; and2-methyl-3-(3-methoxyphenyl)pentanenitrile.5. The compound according to claim 1 , wherein the compound is an intermediate for preparing tapentadol and analogues thereof. This application is a division application of U.S. application Ser. No. 13/884,810 filed on May 10, 2013, which claims the priority right of PCT/CN 2011/001248 filed on Jul. 29, 2011.The invention belongs to the field of pharmaceutical preparation, and relates to a novel intermediate for preparing tapentadol and analogues thereof.Tapentadol hydrochloride is the hydrochloride of tapentadol, and a novel central analgesic with dual mechanism of action developed by Johnson & Johnson Inc. in USA. It is used as medicine in the form of single isomer of (1R,2R), molecular formula: CHClNO, chemical name: (1R,2R)-3-(3-dimethylamino ...

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Номер записи: 77

25-02-2016 дата публикации

PHARMACEUTICALLY ACCEPTABLE AMINE SALTS OF PITAVASTATIN

Номер: US20160052887A1

Автор: De Lange Ben

Принадлежит: DSM SINOCHEM PHARMACEUTICALS NETHERLANDS B.V.

The present invention relates to pharmaceutically acceptable amine salts of pitavastatin and a method for producing pharmaceutically acceptable amine salts of pitavastatin. Also provided are pharmaceutical compositions of these amine salts or solvates thereof, and methods of their use as HMG-CoA reductase inhibitors. 1. A pharmaceutically acceptable amine salt of pitavastatin , wherein said amine is selected from the group consisting of aminopolyols and tetraalkyl ammonium salts.2. The pharmaceutically acceptable amine salt of pitavastatin of wherein said aminopolyol is tromethamine.3. The pharmaceutically acceptable amine salt of pitavastatin of wherein said tetraalkyl ammonium salt is choline.4. A method for the preparation of an amine salt of pitavastatin comprising reacting pitavastatin acid or pitavastatin calcium salt with an amine in a solvent followed by precipitating said amine salt of pitavastatin claim 1 , wherein said reacting is carried out at a first temperature and said precipitating is carried out at a second temperature that is at least 5° C. below said first temperature.6. Method according to wherein said amine is selected from the group consisting of amino acids claim 4 , aminopolyols claim 4 , amino sugars claim 4 , ammonia claim 4 , ethyl amine derivatives claim 4 , guanines claim 4 , purines claim 4 , tetraalkyl ammonium salts and vitamins.7. Method according to wherein said amine is an amino acid selected from the group consisting of histidine claim 6 , lysine and ornithine.8. Method according to wherein said amine is tromethamine.9. Method according to wherein said amine is an amino sugar selected from the group consisting of daunosamine claim 6 , galactosamine claim 6 , glucosamine and N-methylglucamine.10. Method according to wherein said amine is an ethyl amine derivative selected from the group consisting of benzathine claim 6 , diethyl amine claim 6 , ethanol amine claim 6 , ethyl amine claim 6 , ethylene diamine claim 6 , 1-(2- ...

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Номер записи: 78

13-02-2020 дата публикации

PROCESS FOR THE PREPARATION OF l-NOREPINEPHRINE BITARTRATE MONOHYDRATE HAVING HIGH ENANTIOMERIC PURITY

Номер: US20200048185A1

Автор: KADAM Vijay Trimbak, Minhas Gurpreet Singh, Minhas Harpreet Singh, SARANAPU Nareesh, SHAIKH Amin Rashid

Принадлежит:

The present invention, discloses optically pure compounds of l-Norepinephrine and its acid addition salts and hydrates and process for the preparation thereof. Specifically, the present invention discloses optically pure compounds of l-Norepinephrine bitartrate, its process of preparation and pharmaceutical compositions comprising the same. 1. A process for the preparation of optically pure l-Norepinephrine bitartrate monohydrate , wherein the process comprises;a) treating dl-Norepinephrine base with D-(−)-tartaric acid in the presence of water and an organic solvent to obtain crude l-Norepinephrine bitartrate;b) converting the l-Norepinephrine bitartrate obtained in step (a) into l-Norepinephrine base;c) treating the l-Norepinephrine base obtained in step (b) with L-(+)-tartaric acid and water to obtain l-Norepinephrine Bitartrate monohydrate having an optical purity of greater than 99%.2. The process as claimed in claim 1 , wherein step (b) comprises converting the l-Norepinephrine bitartrate obtained in step (a) into l-Norepinephrine base by treating with ammonia.3. The process as claimed in claim 1 , wherein step (b) comprises:a first step of converting the l-Norepinephrine bitartrate obtained in step (a) into l-Norepinephrine base by treating with ammonia;a second step of treating the l-Norepinephrine base obtained in the first step with D-(−)-tartaric acid to obtain pure l-Norepinephrine bitartrate; anda third step of converting the l-Norepinephrine bitartrate obtained in the second step into l-Norepinephrine base by treating with aqueous ammonia solution.4. The process as claimed in claim 1 , further comprising:d) purifying the l-Norepinephrine Bitartrate monohydrate obtained in step (c) from a water/IPA mixture to obtain l-Norepinephrine Bitartrate monohydrate having an optical purity of greater than 99.5%.5. The process as claimed in claim 1 , wherein the organic solvent is selected from the group consisting of methanol claim 1 , ethanol claim 1 , ...

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Номер записи: 79

21-02-2019 дата публикации

A PROCESS FOR PREPARING BETA AGONIST

Номер: US20190055189A1

Автор: REDDY G. Pratap, REDDY M. Kesava

Принадлежит:

Disclosed is a process for preparing β-agonist, 1-(4-amino-3,5-dichlorophenyl)-2-(tert-butylamino) ethanol, of Formula I. The process comprises refluxing 1-(4-amino-3,5-dichlorophenyl) ethanone of Formula II and selenium dioxide in the presence of 1,4-dioxane to form compound of Formula III. Further, compound of Formula III is heated at a temperature below 30° C. in the presence of t-butyl amine to form compound of Formula IV. The compound of Formula IV is treated with sodium borohydride to form compound of Formula I. 2. The process as claimed in claim 1 , wherein the predefined temperature in step c) is in a range of 25° C.-30° C.4. The process as claimed in claim 3 , wherein the predefined temperature in step a) is in a range of 25° C.-70° C.5. The process as claimed in claim 3 , wherein the alcohol used in step a) is isopropyl alcohol.6. The process as claimed in claim 3 , wherein the predefined temperature in step b) is below 30° C.7. The process as claimed in claim 3 , wherein the predefined pH in step b) is in a range of 10-12.9. The process as claimed in claim 8 , wherein the predefined temperature is in a range of 60°-70° C.10. The process as claimed in claim 8 , the predefined pH is in a range of 6-6.5.11. The process as claimed in claim 8 , wherein the solvent is selected from isopropyl alcohol and toluene claim 8 , preferably isopropyl alcohol. The invention relates to a process for preparing β agonist and more particularly, to a process for preparation of Clenbuterol and salts thereof.β-agonists are a class of sympathomimetic agents which act upon the β adrenoceptors that relax muscles of the airways and results in easier breathing.Clenbuterol (CL) is an extremely potent β-agonist with preferential affinity for β2-adrenoceptor of the bronchial and uterine smooth muscle. Clinical trials have however revealed that the selectivity of CL for bronchodilation is not absolute and even at “therapeutic doses” this β-agonist can activate β1-adrenoceptors in the ...

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Номер записи: 80

04-03-2021 дата публикации

PROCESS FOR THE SYNTHESIS OF OPTICALLY ACTIVE BETA-AMINO ALCOHOLS

Номер: US20210061757A1

Автор: Bertolini Giorgio, BERTUOLO Stefania, Colli Corrado, Di Fabio Romano, GARIS Faris, MAIORANA Stefano, NISIC Filippo, RONZONI Silvano, SADA Mara

Принадлежит:

Subject-matter of the present invention is a process for the preparation of optically active phenyl-beta-amino alcohols by means of a specific reduction of the corresponding phenyl-beta-amino ketones. Further subject-matter of the invention are said novel synthesis intermediates and their use for the preparation of active pharmaceutical ingredients. 2. The process according to claim 1 , wherein said protecting groups may be removed by hydrogenation or alkaline hydrolysis.3. The process according to claim 2 , wherein said protecting groups are selected from benzyl and carbobenzyloxy.4. The process according to claim 2 , wherein said protecting groups are removed by hydrogenation with a maximum hydrogen pressure of 3.0±0.2 bar claim 2 , in the presence of a carboxylic acid which has at least one chiral center and is in enantiomerically pure form.5. The process according to wherein said acid is selected from D-tartaric acid claim 4 , L-tartaric acid claim 4 , D-benzoyltartaric acid claim 4 , L-benzoyltartaric acid claim 4 , D-camphor-10-sulfonic acid claim 4 , L-camphor-10-sulfonic acid claim 4 , D-mandelic acid claim 4 , L-mandelic acid.6. The process according to claim 1 , wherein Rand Rare the same; and/or Rand Rdo not both represent hydrogen; and/or Rand Rare the same and each represents a benzyl group.78-. (canceled)9. The process according to claim 1 , wherein Rrepresents a carbobenzyloxy group.10. The process according to claim 1 , wherein Rand Rare the same and each represents a benzyl group and Rrepresents a carbobenzyloxy group.11. The process according to claim 1 , wherein R claim 1 , Rand Rare the same and each represents a carbobenzyloxy group.12. The process according to claim 1 , wherein Ris a carbobenzyloxy group and Ris hydrogen.13. The process according to claim 1 , wherein said alkyl group is selected from methyl and isopropyl.14. The process according to claim 1 , wherein R claim 1 , Rand Rare the same and each represents a carbobenzyloxy group and ...

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Номер записи: 81

22-05-2014 дата публикации

PROCESS FOR PRODUCING AN AMINOPROPYNE OR ENAMINONE

Номер: US20140142304A1

Автор: Lin Zhewang, Yu Dingyi, Zhang Yugen

Принадлежит: AGENCY FOR SCIENCE, TECHNOLOGY AND RESEARCH

There is provided a process for producing an aminopropyne or an enaminone comprising the step of reacting a metal acetylide, an amine and a carbonyl-containing compound in the presence of a transition metal catalyst. There is also provided a process for producing an aminopropyne comprising the step of reacting a metal acetylide, an amine and a halide-containing compound in the presence of a transition metal catalyst at a reaction temperature of 50° C. to 150° C. There are also provided processes to further synthesize the aminopropyne produced to obtain a butyneamine, another aminopropyne or a triazol. 1. A process for producing an aminopropyne comprising the step of reacting a metal acetylide , an amine and a carbonyl-containing compound in the presence of a transition metal catalyst.2. The process as claimed in claim 1 , wherein said aminopropyne has a terminal alkyne group.3. The process as claimed in claim 1 , wherein said metal acetylide has the structure MC claim 1 , where M is a metal selected from the group consisting of an alkali metal claim 1 , an alkaline earth metal and a transition metal; or wherein said metal acetylide is selected from the group consisting of calcium carbide (CaC) claim 1 , lithium acetylide (LiC) and lanthanium acetylide (LaC).4. (canceled)5. The process as claimed in claim 1 , wherein the transition metal of said transition metal catalyst is selected from the group consisting of copper claim 1 , silver and gold; wherein the copper catalyst is selected from the group consisting of copper chloride claim 1 , copper bromide claim 1 , copper iodide claim 1 , copper fluoride claim 1 , copper acetate and copper acetylacetonate.6. (canceled)7. The process as claimed in claim 1 , wherein said carbonyl-containing compound is an aldehyde having the structure RCHO claim 1 , where Ris selected from aryl or C-alkyl claim 1 , said aryl being optionally substituted by at least one of halide claim 1 , nitrile claim 1 , C-alkyl claim 1 , C-alkoxide ...

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Номер записи: 82

28-02-2019 дата публикации

ETHERAMINES BASED ON 1,3-DIALCOHOLS

Номер: US20190062264A1

Автор: Ebert Sophia, Eidamshaus Christian, Hayes Michael Patrick, Henke Karie Marie, LOUGHNANE Brian Joseph, LUDOLPH Bjoern, Nash Jay Frank, SCIALLA Stefano

Принадлежит:

An etheramine mixture comprising of at least one amine selected from the group consisting of amine of Formula (I) and amine of Formula (II) wherein R-Rare independently selected from H, alkyl, cycloalkyi, aryl, alkylaryl, or arylalkyi, wherein at least one of R-Rand at least one of R-Ris different from H, and wherein Z-Zare linear CHCHCHNH. 2. The etheramine mixture according to claim 1 , wherein the etheramine mixture comprises at least 90% by weight claim 1 , based on a total weight of the etheramine mixture claim 1 , of an amine of Formula (I) and/or (II).3. The etheramine mixture according to claim 1 , wherein in said amine of Formula (I) or Formula (II) claim 1 , R claim 1 , R claim 1 , R claim 1 , R claim 1 , R claim 1 , R claim 1 , R claim 1 , and Rare H and R claim 1 , R claim 1 , R claim 1 , and Rare independently selected from C1-16 alkyl or aryl.4. The etheramine mixture according to claim 1 , wherein in said amine of Formula (I) or Formula (II) claim 1 , R claim 1 , R claim 1 , R claim 1 , R claim 1 , R claim 1 , R claim 1 , R claim 1 , and Rare H and R claim 1 , R claim 1 , R claim 1 , and Rare independently selected from a butyl group claim 1 , an ethyl group claim 1 , a methyl group claim 1 , a propyl group claim 1 , or a phenyl group.5. The etheramine mixture according to claim 1 , wherein in said amine Formula (I) or Formula (II) claim 1 , Rand Rare each an ethyl group claim 1 , R claim 1 , R claim 1 , RR claim 1 , R claim 1 , R claim 1 , R claim 1 , Rare each H claim 1 , Rand Rare each a butyl group.6. The etheramine mixture according to claim 1 , wherein the amine of Formula (I) or Formula (II) has a weight average molecular weight of about 150 to about 1000 grams/mol.7. The etheramine mixture according to claim 1 , wherein the amine of Formula (I) or Formula (II) is reacted with an acid.8. A method of using the etheramine mixture of claim 1 , the method comprising using said etheramine mixture in personal care.9. A method of using the etheramine ...

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Номер записи: 83

17-03-2022 дата публикации

METHODS FOR PREPARING AMMONIUM TETRATHIOMOLYBDATE

Номер: US20220081387A1

Автор: Oltner Viveca, Wahlstrom Niklas

Принадлежит: ALEXION PHARMACEUTICALS, INC.

This disclosure relates to crystalline ammonium tetrathiomolybdate having pharmaceutical grade purity and processes for manufacturing crystalline ammonium tetrathiomolybdate. This disclosure also relates to processes for manufacturing bis-choline tetrathiomolybdate having pharmaceutical grade purity. 1. A process for manufacturing crystalline ammonium tetrathiomolybdate (ATTM) , the process comprising:contacting a molybdenum compound selected from ammonium heptamolybdate, ammonium dimolybdate, sodium molybdate, molybdenum oxide, and hydrate thereof with water and ammonia in a reaction vessel under stirring to obtain a molybdenum compound solution;providing ammonium sulfide to the molybdenum compound solution in an amount corresponding to a S:Mo molar ratio in a range of 4.5:1 to 6.5:1 over a period of time sufficient to obtain a reaction mixture;maintaining the reaction mixture at a temperature in a range of 35° C. to 55° C. for a reaction time of at least 4 hours to create a slurry;optionally providing a crystallization solvent to the slurry;optionally maintaining the slurry at a temperature in a range of 10° C. to 30° C. for at least 2 hours; andremoving liquid from the slurry to obtain crystalline ATTM.2. The process of claim 1 , wherein the molybdenum compound is selected from ammonium heptamolybdate claim 1 , ammonium dimolybdate claim 1 , sodium molybdate claim 1 , and hydrate thereof.3. The process of claim 1 , wherein the molybdenum compound is ammonium heptamolybdate or ammonium heptamolybdate tetrahydrate.4. The process of claim 1 , wherein the molybdenum compound is ammonium dimolybdate.5. The process of any one of - claim 1 , wherein ammonium sulfide is provided in an amount corresponding to a S:Mo molar ratio in a range of 4.5:1 to 6.2:1.6. The process of any one of - claim 1 , wherein the period of time sufficient to obtain a reaction mixture is at least 15 minutes.7. The process of any one of - claim 1 , wherein the reaction mixture is maintained at a ...

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Номер записи: 84

10-03-2016 дата публикации

PROCESS FOR CHOLINE HYDROXIDE

Номер: US20160068476A1

Автор: Moonen Kristof, SCHELDEMAN Daan, Ulrichts Dieter

Принадлежит: TAMINCO

Disclosed is a process for the production of choline hydroxide includes reacting at a temperature above 30.0° C. ethylene oxide, trimethylamine, and water in the presence of an aqueous medium in such amounts as to form a diluted choline hydroxide solution having a choline hydroxide concentration of less than 40 wt % and removing at least a portion of the aqueous medium from the diluted choline hydroxide solution to form a concentrated aqueous choline hydroxide solution having a choline hydroxide concentration which is at least 1.05 times the choline hydroxide concentration of the diluted choline hydroxide solution. The process allows for large scale, continuous production of concentrated aqueous choline hydroxide solutions of good quality under economically advantaged consumption factors for ethylene oxide. 120-. (canceled)21. A process for the production of choline hydroxide comprising:a) reacting at a temperature above 30.0° C., in the presence of an aqueous medium, primary reactants comprising ethylene oxide, trimethylamine, and water in such amounts as to form a diluted choline hydroxide solution having a choline hydroxide concentration of at most 38.0 wt %, andb) removing at least a portion of the aqueous medium from the diluted choline hydroxide solution to form a concentrated aqueous choline hydroxide solution having a choline hydroxide concentration which is at least 1.05 times the choline hydroxide concentration of the diluted choline hydroxide solution.22. The process according to claim 21 , wherein the aqueous medium comprises a molar excess of water of 100% to 6000% relative to the stoichiometric amount theoretically required for forming the amount of choline hydroxide in the diluted choline hydroxide solution.23. The process according to claim 21 , wherein a molar excess of trimethylamine is used when reacting the ethylene oxide claim 21 , trimethylamine claim 21 , and water.24. The process according to claim 23 , wherein the molar excess of ...

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Номер записи: 85

27-02-2020 дата публикации

ETHERAMINES PREPARED FROM A MIXTURE OF TWO OR MORE MULTIFUNCTIONAL ALCOHOL INITIATORS, AND THEIR USE AS CURATIVES OR INTERMEDIATES FOR POLYMER SYNTHESIS

Номер: US20200062890A1

Автор: Klein Howard P., Lewis David C., Patterson Leah, Renken Terry L., Zhou Hui

Принадлежит:

Implementations described herein generally relate to etheramine mixtures formed from a mixture of two or more multifunctional alcohol initiators, processes for the etheramine mixtures production, and its use as a curing agent or as a raw material in the synthesis of polymers. In one implementation, the process comprises mixing a polyol initiator having a melting point greater than a processing temperature and a polyol initiator having a melting point less than the processing temperature to form a polyol initiator mixture having a melting point less than the processing temperature, charging the polyol initiator mixture to an alkoxylation reaction zone, contacting the polyol initiator mixture with an alkylene oxide in the alkoxylation reaction zone to provide a mixture of alkoxylated precursor polyols and charging the mixture of alkoxylated precursor polyols to a reductive amination zone and reductively aminating the mixture of alkoxylated precursor polyols to form the etheramine mixture. 1. A composition comprising an etheramine mixture that comprises the reaction product of ammonia and a mixture of alkoxylated precursor polyols;wherein the reaction is conducted under reductive amination reaction conditions;wherein the mixture of alkoxylated polyols is the reaction product of a polyol initiator mixture having a melting point less than a processing temperature with an alkylene oxide; andwherein the polyol initiator mixture comprises a first polyol initiator having a melting point greater than the processing temperature and a second polyol initiator having a melting point less than the processing temperature.5. The composition of claim 1 , wherein the second polyol initiator is neopentyl glycol.6. The composition of claim 5 , wherein the second polyol initiator is selected from the group consisting of: 1 claim 5 ,4-cyclohexanedimethanol claim 5 , 1 claim 5 ,4-butanediol claim 5 , ethylene glycol and combinations thereof.7. The composition of claim 5 , wherein the ...

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Номер записи: 86

29-05-2014 дата публикации

Process for making tertiary aminoalcohol compounds

Номер: US20140145108A1

Автор: Christian Spieker, David W. Moore, John D. Gummere

Принадлежит: ANGUS CHEMIE GMBH

A process for making a tertiary aminoalcohol compound is disclosed. The process comprises using an excess amount of a carbonyl compound in a condensation step between the carbonyl compound and a nitroalkane in the presence of a catalytic amount of a tertiary aminoalcohol compound, and conducting a hydrogenation/alkylation step to produce the tertiary aminoalcohol. The tertiary aminoalcohol compound used to catalyze the condensation step is preferably the same tertiary aminoalcohol compound produced in the hydrogenation/alkylation step. The process uses fewer steps than conventional processes.

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Номер записи: 87

24-03-2022 дата публикации

A PROCESS FOR THE PREPARATION OF ENANTIOMERICALLY PURE NOREPINEPHRINE

Номер: US20220089520A1

Автор: "ZACCHE Matteo", Gatti Pier Andrea, GERLI Fulvio, Rondina Fabio, SBARBADA Davide

Принадлежит: Edmond Pharma, s.r.l.

The invention concerns a new, efficient process for the preparation of enantiomerically pure norepinephrine (also known as noradrenaline), or an addition salt thereof, using a catalytic hydrogenation system under hydrogen donor transfer. The invention also discloses a novel intermediate and the process for the preparation thereof. 2. The process of wherein in the compound of formula III R is selected from the group of hydrogen claim 1 , a carboxyl group claim 1 , an alkyl radical having from of 1 to 17 carbon atoms claim 1 , or an aryl radical of not more than 12 carbon atoms claim 1 , said alkyl claim 1 , cycloalkyl and aryl radical being optionally substituted by a further carboxyl group.3. The process of wherein in step a) in the compound of formula IV X is Cl claim 1 , the solvent is water and the auxiliary base is triethylamine or benzylamine.4. The process of wherein in step a) the carboxylic acid is selected from the group consisting of formic claim 1 , acetic claim 1 , propionic claim 1 , oxalic claim 1 , malonic claim 1 , succinic claim 1 , benzoic claim 1 , toluic claim 1 , o-phthalic and tartaric acid claim 1 , preferably formic acid and acetic acid.5. The process of claim 1 , wherein step b) comprises reacting a compound of Formula III with hydrogen or an hydrogen source in the presence of a suitable catalyst claim 1 , to obtain enantioselectively a compound of Formula V and optionally isolating the compound of Formula V as a free base or acid addition salt thereof.7. The process of claim 6 , wherein in the compounds of formula VI n is 1 and the catalyst is selected from the group of C3-[(S claim 6 ,S)-teth-TsDPEN-RuCl] claim 6 , C3-[(S claim 6 ,S)-teth-MtsDPEN-RuCl] claim 6 , C3-[(S claim 6 ,S)-teth-MesDPEN-RuCl] claim 6 , and C3-[(S claim 6 ,S)-teth-TrisDPEN-RuCl] claim 6 , preferably C3-[(S claim 6 , S)-teth-TsDPEN-RuCl].8. The process of wherein step c) comprises reacting compound of Formula V with hydrogen or a hydrogen source claim 1 , in the ...

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Номер записи: 88

16-03-2017 дата публикации

CLOMIPHENE SYNTHESIS USING A SINGLE SOLVENT

Номер: US20170073302A1

Автор: HSU Kuang, Podolski Joseph S.

Принадлежит: REPROS THERAPEUTICS INC.

The present invention provides a one-pot method for synthesizing clomiphene (a mixture of the isomers cis-clomiphene and trans-clomiphene) utilizing a single solvent. In a preferred embodiment, the single solvent is dichloromethane (DCM, also known as methylene chloride). The present invention provides an improved method for synthesizing clomiphene and purifying clomiphene isomers. 2. The method of claim 1 , wherein the solvent is dichloromethane.3. The method of wherein the mineral acid in step (a) is sulfuric acid.4. The method of claim 1 , wherein the chlorinating agent in step (b) is N-chlorosuccinimide.5. The method of claim 3 , wherein the solution is maintained at a temperature of about 0° C. during addition of the mineral acid in step (a).6. The method of wherein a suitable base is added to the clomiphene solution obtained in step (b) thereby converting clomiphene to the free base form.7. The method of claim 6 , wherein saturated aqueous sodium bicarbonate solution is added to the clomiphene solution obtained in step (b).8. The method of claim 6 , comprising loading the solution comprising clomiphene free base onto a chromatographic column and eluting the column under conditions suitable for obtaining essentially pure trans-clomiphene.9. The method of further comprising recrystallizing the trans-clomiphene.10. A method for preparing essentially pure trans-clomiphene isomer comprising dissolving a desired quantity of 1-{4-[2-(Diethylamino)ethoxy]phenyl}-1 claim 8 ,2-diphenylethanol in a suitable amount of dichloromethane and thereafter(a) adding to the dichloromethane solution a mineral acid in an amount effective to dehydrate the 1-{4-[2-(Diethylamino)ethoxy]phenyl}-1,2-diphenylethanol thereby producing a 2-{4-[(Z)-1,2-diphenylvinyl]phenoxy}-N,N-di ethyl ethanaminium salt; and thereafter(b) adding to the dichloromethane solution N-chlorosuccinimide in an amount effective to chlorinate the 2-{4-[(Z)-1,2-diphenylvinyl]phenoxy}-N,N-diethyl ethanaminium salt ...

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Номер записи: 89

05-03-2020 дата публикации

Method for Preparing Levobunolol Hydrochloride

Номер: US20200071259A1

Автор: Feng Dongxiang, Tao Lianzhi, XU Weiming, Zhang Pengfei

Принадлежит:

The present invention provides a method for preparing levobunolol hydrochloride. In the present invention S-1-tert-butyl-epoxy methylamine is subjected to a substitution reaction with 5-hydroxy-1-tetralone, and acidified to obtain the target product levobunolol hydrochloride. The method provided by the present invention greatly improves the regioselectivity of the reaction, avoids the occurrence of side reactions, and effectively improves the yield and optical purity of levobunolol hydrochloride, with the yield being 87.3%, and the ee value being over 99%. 1. A method for preparing levobunolol hydrochloride , comprising the following steps:mixing 5-hydroxy-1-tetralone with S-1-tert-butyl-epoxymethylamine, an alkaline agent and a solvent, to obtain S-5-(3′-tert-butylamino-2′-hydroxy)-propoxy-3,4-dihydro-1(2H)tetralone through a substitution reaction; andacidifying S-5-(3′-tert-butylamino-2′-hydroxy)-propoxy-3,4-dihydro-1(2H)tetralone to give levobunolol hydrochloride;wherein the method for preparing 5-hydroxy-1-tetralone comprises the following steps:mixing 1,5-dihydroxynaphthalene, a metal catalyst, a reducing agent and an alcohol-water solven to obtain 5-hydroxy-1-tetralone through a reduction reaction;wherein the reducing agent comprises one or more of ammonium formate, sodium formate, potassium formate, formic acid and hydrazine hydrate: and the molar ratio of the reducing agent to 1,5-dihydroxynaphthalene is (1-3):1.2. (canceled)3. The preparation method of claim 2 , wherein the metal catalyst comprises palladium on carbon or raney nickel; and the mass of the metal catalyst is 0.5% to 10% by mass of 1 claim 2 ,5-dihydroxynaphthalene.4. (canceled)5. The preparation method of claim 2 , wherein the alcohol compound in the alcohol-water solvent comprises one or more of methanol claim 2 , ethanol claim 2 , n-propanol claim 2 , isopropanol claim 2 , n-butanol claim 2 , isobutanol and sec-butanol; the mass ratio of the alcohol compound to water in the alcohol-water ...

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Номер записи: 90

05-03-2020 дата публикации

Process for manufacturing hydroxyethyl ethylene amines

Номер: US20200071260A1

Автор: Antoon Jacob Berend Ten Kate, Eike Nicolas Kantzer, Hendrik Van Dam, Ina EHLERS, Karl Fredrik LAKE, Michael Bertil Einar SARNING, Michiel Jozef Thomas RAAIJMAKERS, Rens VENEMAN, Rolf Krister EDVINSSON

Принадлежит: Akzo Nobel Chemicals International BV, Nouryon Chemicals International BV, Rise Research Institutes of Sweden Surface Process and Formulation AB

A process for preparing hydroxyethyl ethylene amines and/or ethylene urea derivatives thereof includes reacting monoethylene glycol with an amine-functional compound having at least two —NH— units, of which at least one is selected from the group of primary amine groups and cyclic secondary amine groups, in the presence of a carbon oxide-delivering agent. The amine-functional compound includes at least one —NH—CH2-CH2-NH— unit, wherein one or more —NH—CH2-CH2-NH— units in the amine-functional compound may be present in the form of piperazine moieties or ethylene urea moieties. The molar ratio of amine-functional compound to monoethylene glycol is in the range of 0.2:1 to 1.5:1 and the molar ratio of carbon oxide-delivering agent to —NH—CH2-CH2-NH— units in the amine-functional compound is at least 0.5:1. The process allows the conversion of monoethylene glycol into ethanol amines in the absence of metals-containing catalysts and without using ammonia.

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Номер записи: 91

18-03-2021 дата публикации

METHOD FOR THE PRODUCTION OF ETHYLENEAMINES

Номер: US20210078935A1

Автор: Bebensee Regine Helga, BECKER Barbara, Heidemann Thomas, KOCH Eva, Luyken Hermann, Melder Johann-Peter

Принадлежит:

The invention relates to a process for preparing alkanolamines and ethyleneamines in the liquid phase, by reacting ethylene glycol and/or monoethanolamine with ammonia in the presence of an amination catalyst which is obtained by reducing a catalyst precursor, wherein the preparation of the catalyst precursor comprises a step a) in which a catalyst precursor comprising one or more catalytically active components of Sn, Cu and Ni is first prepared and the catalyst precursor prepared in step a) is contacted simultaneously or successively with a soluble Ru compound and a soluble Co compound in a step b). 116.-. (canceled)17. A process for preparing alkanolamines and ethyleneamines in the liquid phase , which comprises reacting ethylene glycol and/or monoethanolamine with ammonia in the presence of an amination catalyst which is obtained by reducing a catalyst precursor , wherein the preparation of the catalyst precursor comprises a step a) in which a catalyst precursor comprising one or more catalytically active components of Sn , Cu and Ni is first prepared and the catalyst precursor prepared in step a) is contacted simultaneously or successively with a soluble Ru compound and a soluble Co compound in a step b).18. The process according to claim 17 , wherein the catalyst precursor which is prepared in step a) additionally comprises catalytically active components of Co.19. The process according to claim 18 , wherein the catalyst precursor is prepared by coprecipitation in step a) and claim 18 , before being contacted with Ru and Co in step b) claim 18 , comprises in the range from 1% to 95% by weight of catalytically active components of Sn claim 18 , Cu and/or Ni claim 18 , calculated as CuO claim 18 , NiO and SnO respectively and based in each case on the total mass of the catalyst precursor.20. The process according to claim 18 , wherein the catalyst precursor is prepared by precipitative application in step a) and claim 18 , before being contacted with Ru and Co ...

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Номер записи: 92

23-03-2017 дата публикации

NOVEL BETA-HYDROXYLATED TERTIARY DIAMINES, A PROCESS FOR THEIR SYNTHESIS AND THEIR USE FOR ELIMINATING ACID COMPOUNDS A GASEOUS EFFLUENT

Номер: US20170081275A1

Автор: Delfort Bruno, Grandjean Julien, HUARD Thierry, Le Pennec Dominique, NIGON Armelle, WENDER Aurelie

Принадлежит:

The invention relates to novel nitrogen compounds belonging to the family of tertiary diamines of general formula (I) below, wherein R is an alkanediyl radical —(CH)n- with n=2, 3, 4, 5 or 6. 4. A synthesis method of a nitrogen compound as claimed in claim 1 , comprising the following reactions:a first reaction of epoxidation of an alpha-omega-diene to achieve epoxidation of each one of the alkene functions of the alpha-omega-diene to oxirane functions so as to produce a diepoxyalkane,{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, 'a second reaction of addition of two moles of dimethylamine and one molecule of the diepoxyalkane so as to produce the nitrogen compound as claimed in .'}5. A method as claimed in claim 4 , wherein:the first reaction is an epoxidation reaction of 1,5-hexadiene to produce 1,2,5,6-diepoxyhexane,the second reaction is an addition reaction of two moles of dimethylamine and one molecule of 1,2,5,6-diepoxyhexane to produce N,N,N′,N′-(tetramethyl)-1,6-diamino-2,5-hexanediol.6. A method as claimed in claim 4 , wherein:the first reaction is an epoxidation reaction of 1,7-octadiene to produce 1,2,7,8-diepoxyoctane,the second reaction is an addition reaction of two moles of dimethylamine and one molecule of 1,2,7,8-diepoxyoctane to produce N,N,N′,N′-(tetramethyl)-1,8-diamino-2,7-octanediol.7. A method as claimed in claim 4 , wherein the first epoxidation reaction consists in reacting the alpha-omega-diene with a peracid or a peroxide or a hydroperoxide or oxygen associated with a suitable catalytic system claim 4 , and said peracid can be generated in situ by reaction between a carboxylic acid and a hydrogen peroxide.8. A method as claimed in claim 4 , wherein the second addition reaction is carried out in the presence of excess dimethylamine.9. A method as claimed in claim 4 , wherein the first epoxidation reaction and the second addition reaction are carried out in two successive stages.10. A method of removing acid compounds contained in a ...

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Номер записи: 93

26-03-2015 дата публикации

RHENIUM RECOVERY FROM USED REDUCTIVE AMINATION CATALYSTS

Номер: US20150087837A1

Автор: Hoffman William C., King Stephen W.

Принадлежит:

The present invention provides techniques that selectively recover Re from reductive amination catalysts. In particular, the present invention allows Re to be recovered selectively relative to Ni, Co, and/or Cu, and particularly Ni, that are often present on reductive amination catalysts. The present invention uses a combination of oxidation and extraction techniques to selectively recover Re relative to Ni, Co, and/or Cu. Advantageously, the recovery is selective even when using aqueous solutions for extraction. 1. A method for recovering rhenium from a reductive amination catalyst , comprising the steps of:a) providing a heterogeneous catalyst that has been used in a reducing atmosphere to carry out a reductive amination, wherein the catalyst comprises a substrate and at least one species comprising rhenium and at least one species comprising nickel supported on the substrate, wherein the at least one species comprising rhenium has a first solubility in a liquid carrier, and wherein the substrate comprises at least 15 weight percent alumina based on the total weight of the substrate;b) causing the catalyst to contact the liquid carrier in the presence of heat and at least one oxidizing agent under conditions effective to convert at least a portion of the Re-containing species into a Re-containing product that has a second solubility in the liquid carrier, wherein the second solubility is greater than the first solubility; andc) extracting the Re-containing product into the liquid carrier.2. The method of claim 1 , wherein the substrate comprises a guest/host structure and the heterogenous catalyst is supported at least upon the guest particles.3. The method of claim 1 , wherein step (a) comprises calcining and reducing the substrate.4. The method of claim 1 , wherein the substrate comprises alumina and silica.5. The method of claim 1 , wherein the heterogeneous catalyst further comprises at least one of a Co-containing species and a Cu-containing species.6. The ...

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Номер записи: 94

21-03-2019 дата публикации

METHOD OF PREPARATION OF 4-ISOPROPYLAMINO-1-BUTANOL

Номер: US20190084921A1

Автор: Jia Qiang, Ma Chi, Tang Fanghui

Принадлежит:

The present invention relates to a preparation method of 4-isopropylamino-1-butanol, in which using cheap and readily available tetrahydrofuran and acetic acid solution of hydrogen bromide as starting materials to prepare a novel intermediate of 4-isopropylamino-1-acetoxyl butane and further obtain the target product. The present invention has advantages of convenient process operations, mild reaction conditions, economical and environment-friendly benefits, and suitability for industrial production to obtain the product with high purity and high yield. 1. 4-isopropylamino-1-acetoxyl butane represented by formula (II): The present invention is a divisional application of U.S. application Ser. No. 15/552,772, filed Aug. 22, 2017, which is a U.S. national phase of International Application No. PCT/CN2016/000180 under 35 U.S.C. § 371. The teaching in these related applications are incorporated herein in its entirety by reference.The present invention relates to the technical field of chemical synthesis in pharmaceutical industry, specifically, it relates to a preparation method of 4-isopropylamino-1-butanol and a novel intermediate thereof.4-isopropylamino-1-butanol is an important intermediate in pharmaceutical industry, and its structural formula is represented by formula (I):4-isopropylamino-1-butanol was widely used in the pharmaceutical synthesis, for example, Patent Document WO2002088084A1 disclosed a four-step reaction using 4-isopropylamino-1-butanol as the raw material to prepare pulmonary hypertension drug of selexipag. This document was incorporated by reference into the present application.Journal of Organic Chemistry (1961), Vol. 26, P 1744-1747 disclosed a preparation method of 4-isopropylamino-1-butanol, which comprised: (1) reacted succinic anhydride with isopropyl amine to obtain 3-isopropyl carbamoyl propionic acid; (2) reduced 3-isopropylcarbamoyl propionic acid with lithium aluminum hydride to obtain 4-isopropylamino-1-butanol.This method had ...

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Номер записи: 95

19-03-2020 дата публикации

PROCESS FOR THE CONVERSION OF ETHYLENE OXIDE TO MONOETHANOLAMINE AND ETHYLENEDIAMINE EMPLOYING A ZEOLITE

Номер: US20200087246A1

Автор: BECHTEL Juergen, GORDILLO Alvaro, Gruenanger Christian, KUSCHEL Andreas, LANGE DE OLIVEIRA Armin, LIEBERKNECHT Johannes, Melder Johann-Peter, Müller Ulrich, Parvulescu Andrei-Nicolae

Принадлежит:

The present invention relates to a process for the conversion of ethylene oxide to 2-aminoethanol and/or ethane-1,2-diamme and/or linear polyethylenimines of the formula HN—(CHCHNH)—CHCH—NHwherein n≥1 comprising (i) providing a catalyst comprising a zeolitic material comprising YOand XO, wherein Y is a tetravalent element and X is a trivalent element; (ii) providing a gas stream comprising ethylene oxide and ammonia; (iii) contacting the catalyst provided in (i) with the gas stream provided in (ii) for converting ethylene oxide to 2-aminoethanol and/or ethane-1,2-diamine and/or linear polyethylenimines. 114-. (canceled)15. A process for the conversion of ethylene oxide to 2-aminoethanol and ethane-1 ,2-diamine comprising{'sub': 2', '2', '3, '(i) providing a catalyst comprising a zeolitic material comprising YOand XO, wherein Y is a tetravalent element and X is a trivalent element;'}(ii) providing a gas stream comprising ethylene oxide and ammonia;(iii) contacting the catalyst provided in (i) with the gas stream provided in (ii) for converting ethylene oxide to 2-aminoethanol and ethane-1,2-diamine, wherein in (i) the zeolitic material has the MOR framework structure.16. The process of claim 15 , wherein the gas stream provided in (ii) and contacted with the catalyst in (iii) contains ethylene oxide in an amount in the range of from 0.05 to 10 vol.-%.17. The process of claim 15 , wherein the gas stream provided in (ii) and contacted with the catalyst in (iii) contains ammonia in an amount in the range of from 5 to 90 vol.-%.18. The process of claim 15 , wherein the gas stream provided in (ii) and contacted with the catalyst in (iii) further contains hydrogen in an amount in the range of from 0.1 to 70 vol.-%.19. The process of claim 15 , wherein the gas stream provided in (ii) and contacted with the catalyst in (iii) contains 1 vol.-% or less of hydrogen.20. The process of claim 15 , wherein the gas stream provided in (ii) is heated to a temperature in the range of ...

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Номер записи: 96

07-04-2016 дата публикации

METHOD OF PREPARING INTERMEDIATE OF SALMETEROL

Номер: US20160096816A1

Автор: CHEN Song, Qiu Yinhua, Wu Zhengyuan, Zhang Haoning

Принадлежит:

A method of preparing an intermediate of salmeterol (Compound 1, 2-amino-1-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)ethanol) includes: reacting compound 2 with 2-methoxypropene in a first organic solvent to produce a reaction solution including compound 3, compound 2 including a 2-bromo precursor of Compound 1; reacting compound 3 with a nitrogen source to produce compound 4; reacting compound 4 with sodium borohydride in a second organic solvent to produce compound 5; and debenzylating compound 5 by ammonium formate/palladium-carbon catalytic transfer hydrogenation in a third organic solvent to produce Compound 1. A method of preparing salmeterol includes preparing Compound 1, and reacting Compound 1 to prepare salmeterol. 1. A method of preparing Compound 1 , 2-amino-1-(2 ,2-dimethyl-4H-1 ,3-benzodioxin-6-yl)ethanol , the method comprising:reacting compound 2 with 2-methoxypropene in a first organic solvent to produce a reaction solution comprising compound 3, compound 2 comprising a 2-bromo precursor of Compound 1;reacting compound 3 with a nitrogen source in the reaction solution to produce compound 4;reacting compound 4 with sodium borohydride in a second organic solvent to produce compound 5; anddebenzylating compound 5 by ammonium formate/palladium-carbon catalytic transfer hydrogenation in a third organic solvent to produce Compound 1.2. The method of claim 1 , wherein the first organic solvent comprises tetrahydrofuran claim 1 , dichloromethane claim 1 , acetic ether claim 1 , methyl tert-butyl ether claim 1 , chloroform claim 1 , methyl acetate claim 1 , or a mixture thereof.3. The method of claim 1 , wherein the first organic solvent comprises tetrahydrofuran.4. The method of claim 1 , wherein the reacting of compound 2 with 2-methoxypropene is conducted in the presence of a catalyst.5. The method of claim 4 , wherein the catalyst comprises p-Toluenesulfonic acid.6. The method of claim 1 , wherein the nitrogen source comprises α-phenylethylamine.7. The ...

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Номер записи: 97

12-05-2022 дата публикации

PROCESS FOR PREPARATION OF MIDODRINE AND INTERMEDIATES THEREOF

Номер: US20220144754A1

Автор: DESAI Sanjay Jagdish, Pratap V. Tadikonda, Rupapara Mahesh Laljibhai, SINGH Kumar Kamlesh

Принадлежит:

The invention relates to process for the preparation of midodrine or pharmaceutically acceptable salts thereof. The invention also relates to process for the preparation of intermediates of midodrine. 2. The process according to claim 1 , wherein the reaction at step (a) is performed in the presence of a Lewis acid selected from AlCl claim 1 , AlBr claim 1 , FeCl claim 1 , and FeBr.3. The process according to claim 1 , wherein the reaction at step (b) is performed using potassium phthalimide or sodium phthalimide.4. The process according to claim 1 , wherein the conversion of the compound of Formula (V) into the compound of Formula (IV) at step (c) is performed in the presence of a base or an acid.5. The process according to claim 4 , wherein the base is selected from sodium hydroxide claim 4 , potassium hydroxide claim 4 , lithium hydroxide claim 4 , sodium carbonate claim 4 , potassium carbonate claim 4 , caesium carbonate claim 4 , methylamine claim 4 , ethylamine claim 4 , dimethylamine claim 4 , diethylamine claim 4 , methylethylamine claim 4 , triethylamine claim 4 , ammonium hydroxide claim 4 , and hydrazine hydrate.6. The process according to claim 4 , wherein the acid is selected from hydrochloric acid claim 4 , hydrobromic acid claim 4 , acetic acid claim 4 , trichloroacetic acid claim 4 , and trifluoroacetic acid.7. The process according to claim 1 , wherein the conversion of the compound of Formula (IV) into the compound of Formula (III) at step (c) is performed in the presence of a reducing agent selected from lithium aluminium hydride claim 1 , lithium borohydride claim 1 , sodium borohydride claim 1 , zinc borohydride claim 1 , calcium borohydride claim 1 , sodium cyanoborohydride claim 1 , diisobutylaluminium hydride claim 1 , L-selectride claim 1 , diborane claim 1 , diazene claim 1 , aluminum hydride claim 1 , Red-Al claim 1 , and sodium triacetoxyborohydride.8. The process according to claim 1 , wherein the conversion of the compound of Formula ( ...

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Номер записи: 98

06-04-2017 дата публикации

Production of tea 85% directly without blending with pure cut of dea 99%

Номер: US20170096387A1

Автор: Naeem Alhazmi

Принадлежит: SABIC Global Technologies BV

Systems and methods for producing a triethanolamine product stream with a degree of purity of 85% by weight from the triethanolamine distillation columns in a reactive distillation process without blending the TEA 99 product stream with a pure cut of DEA 99%. The desired triethanolamine product stream can include 85% TEA and 15% DEA and can be created by using a dummy stream at the triethanolamine column via (1) increasing the bottom stream flow rate of the diethanolamine column, and/or (2) reducing the TEA 99 product stream at the triethanolamine column. The bottom stream flow rate at the diethanolamine column can be increased by 80 kilograms per hour and the triethanolamine product stream flow rate can be reduced by 500 kilograms per hour. This process can result in up to a 23 degree temperature reduction in the triethanolamine column, which can improve the color properties of the triethanolamine product.

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Номер записи: 99

06-04-2017 дата публикации

Industrial Process for Making an Ivacaftor and its Intermediates

Номер: US20170096397A1

Автор: DESI REDDY Srinivas Reddy, RANE Dnyandev Ragho, VELIVELA Venkata Srinivasa Rao

Принадлежит:

The present invention relates to an improved process for the preparation of Ivacaftor intermediates. The present invention is also provides industrial applicable, commercially and eco-friendly viable process for the preparation of Ivacaftor 119-. (canceled)2120. The method according to claim , wherein the method comprises producing the compound of formula (II) by a process comprising the steps of:a) reacting aniline with diethyl-2-(ethoxymethylene) malonate;b) treating the product of step a) with Eaton's reagent and heating to 80-90° C.;c) cooling the product of step b) and neutralizing with an alkali carbonate;d) hydrolyzing the product of step c) with an inorganic base; ande) isolating the intermediate of formula (II).22. The method according to claim 21 , wherein the reacting of aniline with diethyl-2-(ethoxymethylene) malonate occurs in absence of a solvent at a temperature ranging from 130-160° for 2-5 hrs.23. The method according to claim 22 , wherein the reacting of aniline with diethyl-2-(ethoxymethylene) malonate occurs at a temperature ranging from 140-150° C. for 2-3 hrs to obtain a compound of formula (V).24. The method according to claim 23 , wherein the compound of formula (V) is further treated with Eaton's reagent to get a cyclized compound of formula (IV).)24. The method according to claim 24 , wherein the compound of formula (IV) is hydrolyzed in presence of the inorganic base to give a 4-Oxo-1 claim 24 , 4-dihydro-quinoline-3-carboxylic acid of formula (II).26. The method according to claim 21 , wherein the alkyl chloroformate is selected from ethyl chloroformate claim 21 , methyl chloroformate (or) isopropyl chloroformate.27. The method according to claim 21 , wherein the inorganic base is selected from sodium hydroxide claim 21 , calcium hydroxide and potassium hydroxide.2820. The method according to claim claim 21 , wherein the method comprises producing the compound of formula (III) by the process comptising the steps of:a) reacting 2,5 di- ...

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Номер записи: 100