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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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Форма поиска

Поддерживает ввод нескольких поисковых фраз (по одной на строку). При поиске обеспечивает поддержку морфологии русского и английского языка
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Применить Всего найдено 9044. Отображено 100.
12-01-2012 дата публикации

Acid-free quaternized nitrogen compounds and use thereof as additives in fuels and lubricants

Номер: US20120010112A1
Принадлежит: BASF SE

The present invention relates to novel acid-free quaternized nitrogen compounds, to the preparation thereof and to the use thereof as a fuel and lubricant additive, more particularly as a detergent additive, as a wax antisettling additive (WASA) or as an additive for reducing internal diesel injector deposits (IDID); to additive packages which comprise these compounds; and to fuels and lubricants thus additized. The present invention further relates to the use of these acid-free 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.

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23-02-2012 дата публикации

Intermediates in the enantioselective synthesis of 3-(aminomethyl)-5-methyl-hexanoic acid

Номер: US20120046468A1

(S)-(+)-3-(aminomethyl)-5-methyl-hexanoic acid or (S)-pregabalin is an anticonvulsive drug. In addition to its use as an anticonvulsive agent, pregabalin has also been indicated as a medicament in the treatment of anxiety, neuropathic pain and pain in patients with fibromyalgia. Provided herein are thioester intermediates in the synthesis of and processes for the synthesis of 3-(aminomethyl)-5-methyl-hexanoic acid in the (R) or (S) configuration.

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29-03-2012 дата публикации

Process for the preparation of cilastatin and sodium salt

Номер: US20120078009A1

An improved process for preparing Cilastatin Sodium including dissolving Cilastatin acid in a solvent using an organic base, adding sodium salt of a week acid and isolating Cilastatin Sodium.

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12-04-2012 дата публикации

Process for the preparation of a iodinating agen

Номер: US20120088926A1
Принадлежит: BRACCO IMAGING SPA

The present invention describes a process for the synthesis of a iodinating agent, being said iodinating agent iodine chloride (ICI.) In particular, the present invention relates to a process for the electrochemical preparation of ICI, as a useful iodinating agent in the preparation of iodinated organic compounds for use as contrast agents or their precursors in the synthesis of the same.

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19-07-2012 дата публикации

Reduction of fused bicyclic impurities in triiodinated x-ray contrast media

Номер: US20120184773A1
Принадлежит: Mallinckrodt LLC

The present disclosure generally relates to an improved process for alkylating a triiodo-substituted arylamide to form a compound suitable for use as an X-ray contrast agent. More particularly, the present disclosure is directed to such a process that limits the formation of fused bicyclic impurities, such as Impurity G, in the alkylation reaction mixture.

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26-07-2012 дата публикации

Hydrochlorination of electron-deficient alkenes

Номер: US20120190879A1
Автор: Michael Todd Coleman
Принадлежит: Future Fuel Chemical Co

The present invention pertains to a method for the hydrochlorination of electron deficient alkenes, particularly alkenes having the functional groups COOH, CONH 2 , and CN. Specific alkenes discussed include acrylic acid, crotonic acid, methacrylic acid, acrylonitrile, acrylamide, and methacrylonitrile. The alkene is combined with a primary or secondary alcohol (e.g., isopropanol) and an acid chloride (e.g., acetyl chloride) under conditions suitable to chlorinate the alkene. Products formed by the invention include 3-chorosubstituted carbonyl compounds such as 3-chlorpropionic acid (3-CPA), 3-chloropropionamide (3-CPAD), and 3-chloropropionitrile among other products.

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23-08-2012 дата публикации

Viral polymerase inhibitors

Номер: US20120214783A1
Принадлежит: BOEHRINGER INGELHEIM INTERNATIONAL GMBH

Compounds of formula I: wherein X, R 2 , R 3 , R 3a , R 3b , R 5 and R 6 are defined herein, are useful as inhibitors of the hepatitis C virus NS5B polymerase.

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08-11-2012 дата публикации

Intermediate compounds and processes for the preparation of tapentadol and related compounds

Номер: US20120283463A1
Принадлежит: Mapi Pharma Ltd

The present invention discloses processes for the preparation of 3-[(1R,2R)-3-(dimethyl-amino)-1-ethyl-2-methyl-propyl]phenol (Tapentadol), salts thereof and related compounds of formula (A), including stereoisomers and pharmaceutically acceptable salts thereof, and to certain intermediates used in such process.

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27-12-2012 дата публикации

Bis-phosphate compound and asymmetric reaction using the same

Номер: US20120330038A1
Принадлежит: API Corp, Tohoku University NUC

A novel bis-phosphate compound is provided which can be applied to a wide range of reactive substrates and reactions as an asymmetric reaction catalyst and can realize an asymmetric reaction affording a high yield and a high enantiomeric excess. The bis-phosphate compound has a tetraaryl skeleton represented by General Formula (1). In an asymmetric reaction, an amidodiene and an unsaturated aldehyde compound are reacted with each other in the presence of the optically active bis-phosphate compound to give an optically active amidoaldehyde. The invention allows a reaction such as an asymmetric Diels-Alder reaction to proceed efficiently, which has been difficult with conventional mono-phosphate compounds. Thus, the invention enables an industrially feasible method for the production of optically active amidoaldehydes, optically active β-amino acid derivatives, optically active diamine compounds, optically active pyrrolidine derivatives and optically active dihydropyran derivatives which are useful as products such as medicines, agricultural chemicals and chemical products as well as synthesis intermediates for such products.

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03-01-2013 дата публикации

Agomelatine hydrochloride hydrate and preparation thereof

Номер: US20130005820A1
Принадлежит: Laboratoires Servier SAS

The present invention relates to an agomelatine hydrochloride hydrate of formula I, preparation and use thereof, and to pharmaceutical composition containing it. The agomelatine hydrohalide hydrate obtained through the present method has significant increased solubility than agomelatine, and therefore is more suitable for manufacturing pharmaceutical formulations. In addition, the product enjoys higher stability and purity. Using the present method, product of high purity can be obtained through a simple process, free of any complicated steps. wherein X is Cl.

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31-01-2013 дата публикации

Process for the preparation of lacosamide

Номер: US20130030216A1
Принадлежит: EUTICALS SPA

A novel process for the synthesis of Lacosamide using D,L-serine as starting material is described, where the methylation reaction of hydroxyl is carried out using an inexpensive base such as NaOH and an inexpensive alkylating agent, non-toxic and non-carcinogenic, such as methyl p-toluenesulfonate; the R enantiomer is isolated from the racemic mixture of Lacosamide after selective hydrolysis of the acetamide, salification of the racemic mixture with a chiral acid (HX*) in an organic solvent, resolution of the diastereoisomeric mixture, preferably by precipitation of the R enantiomer, and subsequent acetylation of the optically pure intermediate.

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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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21-03-2013 дата публикации

Process for Producing Aliskiren

Номер: US20130071899A1
Принадлежит: Chemo Iberica SA

A new route of synthesis of the compound Aliskiren of formula (I), used in the treatment of hypertension, is described.

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21-03-2013 дата публикации

18ß-GLYCYRRHETINIC ACID DERIVATIVES AND SYNTHETIC METHOD THEREOF

Номер: US20130072694A1
Принадлежит: KAOHSIUNG MEDICAL UNIVERSITY

The present invention provides a chemical compound having the structure being one selected from a group consisting of 2. The method according to further comprising a step of using an isopropylamine solution as the amine solution when Ris CONHCH(CH) claim 1 , and using an aniline solution as the amine solution when Ris CONHCH.3. The method according to further comprising steps of:methylating the 18β-glycyrrhetinic acid to obtain a methylated 18β-glycyrrhetinic acid; andoxidizing the methylated 18β-glycyrrhetinic acid to obtain a second compound.4. The method according to further comprising a step of esterifying the lactone compound to obtain a first derivative of the lactone compound.5. The method according to further comprising a step of cleaving a lactone ring of the lactone compound to obtain a second derivative of the lactone compound.6. The method according to further comprising a step of treating the second derivative with an alcohol solution to obtain a third derivative of the lactone compound.7. The method according to claim 6 , wherein the alcohol solution is one of an isopropyl alcohol solution and a benzyl alcohol solution.8. The method according to further comprising a step of esterifying the second compound with an alcohol solution to obtain a fourth derivative of the lactone compound.9. The method according to further comprising a step of cleaving a lactone ring of the fourth derivative by an acidic solution to obtain a fifth derivative of the lactone compound.13. The method according to claim 12 , wherein the chemical compound with Rbeing one of CONHCH(CH)and CONHCHis obtained by steps of:oxidizing the 18β-glycyrrhetinic acid to form a first compound;treating the first compound with an m-chloroperbenzoic acid to afford a lactone compound; andtreating the lactone compound with an amine solution to obtain the chemical compound being a first derivative of the chemical compound.14. The method according to further comprising a step of using an ...

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21-03-2013 дата публикации

ENANTIOMERICALLY PURE AMINES

Номер: US20130072711A1
Принадлежит: NABRIVA THERAPEUTICS AG

A compound of formula 3. A compound according to claim 1 , wherein PROT and PROT′ together with the nitrogen atom to which are attached form phthalimido-N-yl.4. A compound according to claim 1 ,wherein PROT″ is benzoyl or trityl.7. A compound according to claim 1 , selected from the group consisting of:{(1R,2R,4R)-4-[(tert-Butoxycarbonyl)-amino]-2-hydroxy-cyclohexyl}-benzene-carbothioate,{(1R,2R,4R)-4-[(2,2,2-Trifluoro-acetyl)-amino]-2-hydroxy-cyclohexyl}-benzene-carbothioate,tert-Butyl [(1R,3R,4R)-3-hydroxy-4-tritylsulfanyl-cyclohexyl]-carbamate, and2,2,2-Trifluoro-N-((1R,3R,4R)-3-hydroxy-4-tritylsulfanyl-cyclohexyl)-acetamide.10. A compound of formula II claim 9 , II claim 9 , IIor IIaccording to claim 9 , selected from the group consisting oftert-Butyl (1R,3R,6R)-(7-oxa-bicyclo[4.1.0]hept-3-yl)-carbamate, and2,2,2-Trifluoro-N-(1R,3R,6S)-(7-oxa-bicyclo[4.1.0]hept-3-yl)-acetamide.12. A process according to claim 11 , wherein none of the intermediates obtained in a) to d) is isolated.13. A process according to claim 11 , wherein the reaction a) to e) is performed in a single solvent (system).14. (canceled) The present invention relates to enantiomerically pure amines, such as amino and thio protected hydroxy-mercapto-cyclohexyl amines and production processes thereof.Organic compounds, such as cyclohexyl amines containing an asymmetric carbon atom may exist in the form of enantiomers, diastereoisomers and mixtures thereof, e.g. racemates. Such compounds may exist in the (R)-, (S)- or (R,S)-configuration. For pharmaceutical use it is often vital to have an active compound comprising an asymmetric carbon atom in one of the enantiomerically pure forms, since one isomer may differ, e.g. in several aspects from another isomer, e.g. one isomer may be more active than the other isomer. Separation of isomers is often burdensome. Chromatography which, for example, may be useful for isomeric separation, is on technical scale not easy to carry out and often needs sophisticated ...

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21-03-2013 дата публикации

Process For The Iodination Of Phenolic Derivatives

Номер: US20130072719A1
Принадлежит: BRACCO IMAGING S.P.A.

The present invention relates to a process for the preparation of iodinated phenols; in particular; it relates to a process including the direct iodination, with suitably activated iodine, of 3,5-disubstituted phenol compounds to the corresponding 3,5-disubstituted-2,4,6-triiodophenols, which are useful intermediates for the synthesis of x-ray contrast media, and to the preparation of the contrast media themselves. 2. The process of wherein claim 1 , within the compounds of formulae 1 and 2 claim 1 , R and R′ represent claim 1 , independently claim 1 , a group of formula —NHRor —NRRwherein each R claim 1 , Rand Ris claim 1 , independently claim 1 , a straight or branched C-Calkyl group optionally substituted by one to three hydroxyl groups.3. The process of wherein claim 2 , within the compounds of formulae 1 and 2 claim 2 , R and R′ represent claim 2 , independently claim 2 , a group selected from:{'sub': '3', '—NHCH,'}{'sub': 2', '2, '—NHCH—CH(OH)—CHOH,'}{'sub': 2', '2, '—NHCH(CHOH), and'}{'sub': 3', '2', '2, '—N(CH)—CH—CH(OH)—CHOH.'}4. The process of wherein the molar ratio between molecular iodine and 3 claim 1 ,5-disubstituted phenol substrate 1 [I/1] is comprised from 1.1 to 1.3 claim 1 , and the molar ratio between iodic acid and 3 claim 1 ,5-disubstituted phenol substrate 1 is comprised from 0.4 to 0.8.5. The process according to wherein the triiodination of the 3 claim 4 ,5-disubstituted phenol substrate 1 with iodine and iodic acid is carried out by using a molar ratio 3 claim 4 ,5-disubstituted phenol substrate:iodine:iodic acid of 1:1.2:0.6.6. The process according to wherein said aqueous medium is water or an aqueous solution.7. The process of comprising: obtaining an aqueous solution of 3 claim 6 ,5-di-substituted phenol substrate of formula 1 claim 6 , or of a salt thereof claim 6 , and adding Iand HIOto said aqueous solution.8. The process according to wherein said aqueous solution of 3 claim 7 ,5-di-substituted phenol substrate is a crude solution ...

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28-03-2013 дата публикации

Process for preparing eddn and edmn

Номер: US20130079492A1
Принадлежит: BASF SE

A process for preparing EDDN and/or EDMN by conversion of FA, HCN and EDA, the reaction being effected in the presence of water, and, after the conversion, water being depleted from the reaction mixture in a distillation column, which comprises performing the distillation in the presence of an organic solvent which has a boiling point between water and EDDN and/or EDMN at the distillation pressure existing in the column or which forms a low-boiling azeotrope with water.

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28-03-2013 дата публикации

SILVER-CATALYZED SYNTHESIS OF AMIDES FROM AMINES AND ALDEHYDES

Номер: US20130079556A1
Принадлежит:

The invention provides a method for producing amides via the reaction of aldehydes and amines with oxygen adsorbed on a metallic silver or silver alloy catalyst. An exemplary reaction is shown in Scheme 1 : (I), (II), (III) 1. A method for preparing an amide comprising reacting an aldehyde and a primary or secondary amine with oxygen adsorbed on a catalyst comprising silver metal or an alloy thereof to produce the amide.4. The method of claim 2 , wherein Rand Rare methyl.5. The method of claim 1 , wherein the aldehyde is formaldehyde.6. The method of claim 1 , wherein the silver alloy is an alloy of silver and gold.7. The method of claim 1 , wherein the source of the adsorbed oxygen is oxygen gas.8. The method of claim 1 , wherein the amine is a primary amine.9. The method of claim 1 , wherein the amine is a secondary amine.10. The method of claim 1 , wherein the catalyst is promoted by a material selected from the group consisting of metal halides claim 1 , carbonates claim 1 , sulfites claim 1 , sulfates claim 1 , nitrites claim 1 , and nitrates claim 1 , transition metal oxoanions claim 1 , lanthanides claim 1 , and alkali and alkaline earth metals.11. The method of claim 1 , wherein the temperatures is from 270 to 1000 K.12. The method of claim 1 , wherein the pressure is from 0.1 atm to 5 atmospheres.13. The method of claim 1 , wherein the catalyst is carried on an inert supporting material. This application claims benefit of U.S. Provisional Application No. 61/336,673, filed Jan. 25, 2010, which is hereby incorporated by reference.This invention was made with U.S. government support under National Science Foundation awards CHE-0513936, PHY-0646094, CHE-0545335, DMR-0820484 and Department of Energy award DE-FG02-84ER13289. The U.S. Government has certain rights in the invention.The invention is in the field of synthetic organic chemistry, and relates specifically to chemical processes involving catalysis, oxidation, and amide synthesis.Amidation is a ...

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18-04-2013 дата публикации

REDUCTION OF ALDEHYDES AND KETONES TO ALCOHOLS

Номер: US20130096317A1
Принадлежит:

The embodiments described herein provide a reduction of an aldehyde or a ketone, such as a Meerwein-Ponnorf-Verley (MPV) reaction of an aldehyde or ketone. In some embodiments, the reaction occurs in the presence of Al[OC(CH)]. In some embodiments, the reaction occurs in the presence of an aprotic solvent. In some embodiments, the aldehyde or ketone is an amino aldehyde or an amino ketone wherein the amine is group is protected such that the nitrogen of the amine has no proton. Other embodiments related to compositions and compounds related to the reduction reaction, or to the preparation or use of the aldehyde, the ketone, or the resulting alcohol. 1. A method of reducing a C═O of an aldehyde or a ketone to a CH—OH of a product alcohol comprising reacting the aldehyde or ketone in the presence of Al[OC(CH)] and a reactant alcohol which comprises a carbon atom directly bonded to both a hydroxyl group and a hydrogen atom2. A method of reducing a C═O of an aldehyde or a ketone to a CH—OH of a product alcohol comprising reacting the aldehyde or ketone in the presence of: Al(OR) , a reactant alcohol comprising a carbon atom directly bonded to both a hydroxyl group and a hydrogen atom , and an aprotic solvent , wherein each Ris independently Calkyl or optionally substituted aryl.3. The method of claim 2 , wherein the aprotic solvent comprises ethyl acetate claim 2 , tetrahydrofuran claim 2 , toluene claim 2 , dichloromethane claim 2 , or an ether.4. The method of claim 2 , wherein the volume ratio of the aprotic solvent to the reactant alcohol is at least about 1:1.7. The method of claim 5 , wherein Ris COR.12. The method of claim 11 , wherein the ratio of diastereomer 1 to diastereomer 2 is at least about 0.5.13. The method of claim 11 , wherein the ratio of diastereomer 1 to diastereomer 2 has a value in the range of about 1 to about 10 claim 11 ,000. 1. Field of the InventionThe embodiments disclosed herein relate to reduction of an aldehyde or ketone, such as by ...

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25-04-2013 дата публикации

PROCESS FOR PREPARING FORMAMIDES AND FORMIC ESTERS

Номер: US20130102807A1
Принадлежит: BASF SE

A process for preparing carboxylic acid derivatives of the formula H—(C═O)—R, R is ORor NRR, Ris optionally substituted C-C-alkyl, C-C-cycloalkyl, C-C-heterocyclyl, C-C-aryl or C-C-heteroaryl, substituents are C-C-alkyl, C-C-alkoxy, C-C-cycloalkyl or C-C-aryl; Rand Rare independently hydrogen or optionally substituted C-C-alkyl, C-Ccycloalkyl, C-C-heterocyclyl, C-C-aryl or C-C-heteroaryl, substituents are selected from the group consisting of C-C-alkyl, C-C-cycloalkyl and C-C-aryl or Rand Rtogether with the nitrogen atom form a five- or six-membered ring which optionally comprises one or more heteroatoms selected from O, S and N and bearing the substituent R, Ris hydrogen or C-C-alkyl; by reacting a reaction mixture comprising carbon dioxide, hydrogen and an alcohol of the formula R—OH or an amine of the formula NHRRin the presence of a catalyst comprising gold at a pressure from 0.2 to 30 MPa and a temperature from 20 to 200° C. in a hydrogenation reactor. 114.-. (canceled)15. A process for preparing carboxylic acid derivatives of the general formula (Ia){'br': None, 'H—(C═O)—R\u2003\u2003(Ia),'}where{'sup': 1', '2', '3, 'R is selected from the group consisting of ORand NRR, where'}{'sup': '1', 'sub': 1', '15', '5', '10', '5', '10', '5', '10', '5', '10, 'claim-text': {'sub': 1', '15', '1', '6', '5', '10', '5', '10, 'where the substituents are selected from the group consisting of C-C-alkyl, C-C-alkoxy, C-C-cycloalkyl and C-C-aryl;'}, 'Ris unsubstituted or at least monosubstituted C-C-alkyl, C-C-cycloalkyl, C-C-heterocyclyl, C-C-aryl or C-C-heteroaryl,'}{'sup': 2', '3, 'sub': 1', '15', '5', '10', '5', '10', '5', '10', '5', '10, 'claim-text': [{'sub': 1', '15', '5', '10', '5', '10, 'where the substituents are selected from the group consisting of C-C-alkyl, C-C-cycloalkyl and C-C-aryl'}, 'or', {'sup': 2', '3', '4, 'Rand Rtogether with the nitrogen atom form a five- or six-membered ring which optionally additionally comprises one or more heteroatoms selected from ...

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02-05-2013 дата публикации

PHENYL-N-ACYL DERIVATIVES OF AMINES AND AMINO ACIDS, A PROCESS FOR THE PREPARATION THEREOF, A PHARMACEUTICAL COMPOSITION AND USE THEREOF

Номер: US20130109880A1

The present invention relates to novel phenyl-N-acyl derivatives of biogenic amines and amino acids of general formula (I) as cyclooxynease inhibitors, possessing analgetic and anti-inflammatory properties and devoid of side effects in particular ulcerogeneity and pro-spasmodic actions, as well as capability to potentiate effect of other analgetics, and possessing in addition antihypoxic, antidepressant and anti-Parkinsonistic action; as well as to the processes for the preparation novel and known phenyl-N-acyl derivatives of biogenic amines, to a pharmaceutical composition and to an agent comprising compounds of general formula (I) as well as to use thereof and a method of treating. 2. The process according to claim 1 , wherein 1-1.2 equivalents of diphenylphosphorylazide and triethylamine are used.3. The process according to claim 1 , wherein as amino derivatives tyrosine or phenylalanine esters are used.43. The process according to any one of - claims 1 , wherein as an organic solvent N claims 1 ,N-dimethylformamide or ethylacetate are used.53. The process according to any one of - claims 1 , which is conducted at the temperature ranging from −25° C. to 0° C.7. The process according to claim 6 , wherein as amino derivatives tyrosine or phenylalanine esters are used. This application is a divisional of co-pending U.S. application Ser. No. 11/886,965, filed on Oct. 23, 2008, which is a U.S. National Stage application under 35 U.S.C. §371 of International Application PCT/RU2006/000139 (published as WO 2006/101422 A1), filed Mar. 24, 2006, which claims priority to Application RU 2005108492, filed Mar. 25, 2005. Benefit of the filing date of each of these prior applications is hereby claimed. Each of these prior applications is hereby incorporated by reference in its entirety.The present invention relates to the field of bioorganic chemistry and concerns novel compounds, phenyl-N-acyl derivatives of biogenic amines as well as a process for synthesis of novel and known ...

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16-05-2013 дата публикации

Process for preparation of lacosamide and some n-benzyl-propanamide intermediate derivatives

Номер: US20130123522A1
Принадлежит: Indoco Remedies Ltd

The present invention discloses novel process for the preparation of (2R)-2-acetamido-N-benzyl-3-methoxypropanamide of Formula I involving novel intermediates of Formula-XIX and Formula-XX.

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16-05-2013 дата публикации

PROCESS FOR THE PREPARATION OF LACOSAMIDE

Номер: US20130123537A1
Принадлежит:

The present invention relates to an improved process for the preparation of Lacosamide of Formula (I), comprising: O-methylating a compound of Formula (V) or a compound of Formula (XX) or a compound of Formula XXII; in the presence of a methylating agent and a base to produce Lacosamide of Formula (I). 2. The process according to claim 1 , wherein the methylating agent used in O-methylation step is selected from methyl iodide claim 1 , methyl chloride claim 1 , methyl bromide claim 1 , methyl fluoride claim 1 , dimethyl sulfate claim 1 , trimethyl silyldiazomethane claim 1 , dimethyl sulfoxide (DMSO) or mixtures thereof.3. The process according to claim 1 , wherein the base used in O-methylation step is selected from sodium hydroxide claim 1 , potassium hydroxide claim 1 , sodium carbonate claim 1 , potassium carbonate claim 1 , sodium bicarbonate claim 1 , potassium bicarbonate or mixtures thereof.4. The process according to claim 1 , wherein the O-methylation is carried out in the presence of a solvent selected from tetrahydrofuran (THF) claim 1 , dichloromethane (MDC) claim 1 , dimethyl sulfoxide (DMSO) claim 1 , acetonitrile (MeCN) claim 1 , ethyl acetate claim 1 , acetone claim 1 , monoglyme claim 1 , diglyme or mixtures thereof.5. The process according to claim 1 , wherein the O-methylation is optionally carried out in the presence of a phase transfer catalyst (PTC) selected from tetraethylammonium-p-toluenesulfonate claim 1 , tetrapropylammonium trifluoromethane sulfonate claim 1 , tetraphenylphosphonium hexafluoroantimonate claim 1 , acetylpyridinium bromide claim 1 , triphenylmethyl triphenylphosponium chloride claim 1 , benzyltriethylammonium chloride claim 1 , benzyltrimethylammonium chloride claim 1 , benzyltriphenylphosphonium chloride claim 1 , benzytributylammonium chloride claim 1 , butyltriethylammonium bromide claim 1 , butyltriphenylphosphonium bromide claim 1 , cetyltrimethyl ammonium bromide claim 1 , cetyltrimethyl ammonium chloride claim 1 , ...

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23-05-2013 дата публикации

NOVEL CATIONIC AMPHIPHILES WITH MANNOSE-MIMICKING HEAD-GROUPS AND A PROCESS FOR THE PREPARATION THEREOF

Номер: US20130129758A1

The present invention discloses novel cationic amphiphiles containing mannose-mimicking shikimic and quinic acid head-groups and a process for preparing cationic amphiphiles with mannose-mimicking polar head-groups such as, shikimic and quinic acids. The findings described herein also demonstrate that compounds of the present invention can target model DNA vaccines to antigen presenting cells (APCs) such as macrophages and dendritic cells (DCs), via mannose receptors expressed on the cell surface of APCs. The cationic amphiphiles disclosed herein show enhanced cellular and humoral immune response compared to their mannosyl counterpart in dendritic cell (DC, the most professional APC) based genetic immunization in mice. Cationic amphiphiles with mannose-mimicking quinic and shikimic acid head-groups described in the present invention are likely to find future applications in the field of genetic immunization. 3. The cationic amphiphile of claim 1 , wherein lipophilic Rand Rmoiety is selected from the group consisting of saturated C-Calkyl groups and unsaturated C-Calkenyl groups containing 1 claim 1 , 2 or 3 double bonds.5. The process of claim 4 , wherein saturated or unsaturated aliphatic hydrocarbon chains of said amine have 8-22 carbon atoms.6. The process of claim 4 , wherein the polar aprotic solvent used in step (a) is selected from the group consisting of dichloro methane (DCM) claim 4 , dimethyl formamide (DMF) claim 4 , dimethylsulfoxide claim 4 , pyridine claim 4 , and triethyl amine.7. The process of claim 4 , wherein quaternization of the intermediate hydrophobic amide obtained in step (a) is carried out at a temperature between 25-30° C.8. The process of claim 4 , wherein the organic solvent used as polar eluent in step (c) is selected from the group consisting of methanol claim 4 , ethanol claim 4 , chloroform claim 4 , dichloro methane and ethyl acetate.9. The process of claim 4 , wherein the halide ion exchange resins used in step (c) is selected ...

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23-05-2013 дата публикации

PROCESSES AND INTERMEDIATES FOR PREPARING STERIC COMPOUNDS

Номер: US20130131359A1
Принадлежит: VERTEX PHARMACEUTICALS INCORPORATED

This invention relates to processes and intermediates for the preparation of an alpha-amino beta-hydroxy acid of Formula 1 2. The process of claim 1 , wherein R claim 1 , is C-Calkyl claim 1 , R′is H and R′is —NHRwherein Ris C-Calkyl or C-Ccycloalkyl.3. The process of claim 2 , wherein Ris propyl and Ris cyclopropyl.5. The process of claim 4 , wherein the aminating reagent is an azide salt and the intermediate azido compound is reduced by hydrogenation.7. The process of claim 6 , wherein the oxidizing reagent is t-butyl hydroperoxide.8. The process of claim 6 , wherein the oxidizing reagent includes a chiral reagent.9. The process of claim 8 , wherein the oxidizing reagent is a mixture of samarium (III) isopropoxide claim 8 , triphenyl arsine oxide claim 8 , S-(−)1 claim 8 ,1′-bi-2-naphthol and 4 Å molecular sieves.10. The process of claim 6 , wherein the oxidizing reagent is urea-hydrogen peroxide in the presence of trifluoroacetic anhydride.11. The process of claim 6 , wherein R′is —OE.12. The process of claim 6 , wherein Ris —NHR.13. The process of claim 11 , further comprising hydrolyzing the compound of Formula ii to give an acid and then converting the acid to an amide compound of Formula ii wherein R′is —NHR.15. The process of claim 14 , wherein the compound of Formula 1 is (2S claim 14 ,3S)-3-amino-N-cyclopropyl-2-hydroxyhexanamide.16. The process of claim 14 , wherein the organic acid is L-tartaric acid.17. The process of claim 14 , wherein the organic acid is deoxycholic acid.18. A compound which is N-cyclopropyl-3-propyloxirane-2-carboxamide.19. A compound which is N-cyclopropyl-3-propyloxirane-2-carboxamide.20. A compound which is 3-azido-N-cyclopropyl-2-hydroxyhexanamide.21. A compound which is 3-amino-N-cyclopropyl-2-hydroxyhexanamide claim 14 , L-tartaric acid salt.22. A compound which is 3-amino-N-cyclopropyl-2-hydroxyhexanamide claim 14 , deoxycholic acid salt. This application claims the benefits of U.S. Provisional Application Ser. No. 60/782,976, ...

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23-05-2013 дата публикации

Process For The Preparation Of Contrast Agents

Номер: US20130131382A1
Принадлежит: BRACCO IMAGING S.P.A.

The present invention relates to a process for the preparation of 5-[(2-hydroxyacyl)amino]-2,4,6-triiodo-1,3-benzendicarboxamidic derivatives comprising the Smiles rearrangement of a suitable precursor, by contact of an aqueous solution of this latter with an anion exchanger solid phase. 4. The process according to claim 1 , wherein the anion exchanger solid phase is a weak anion exchanger resin or a strong anion exchanger resin.5. The process according to any one of or claim 1 , wherein the anion exchanger solid phase is selected from: Amberlite® IRA 400 and Purolite® A830.6. The process according to wherein the aqueous solvent is water.7. The process according to claim 1 , wherein the pH of the reaction is comprised from 6 to 9.9. The process according to claim 8 , wherein the compound of formula (3) is:(R)-2-[[(4-nitrophenyl)sulfonyl)]oxy]propanamide; or2-[[(4-notrophenyl)sulfonyl)]oxy]ethanamide.10. The process according to any one of or claim 8 , wherein the solvent is a mixture of water/dioxane in a ratio of 3:1 by weight. The present invention relates in general to a process for the preparation of 5-[(2-hydroxyacyl)amino]-2,4,6-triiodo-1,3-benzendicarboxamidic derivatives, useful as contrast agents in diagnostic techniques.Contrast agents or contrast media, are substances that can alter the way in which a region is analyzed in medical imaging. In particular, they are able to change the contrast of an organ, an injury, or any other surrounding structure, to make visible such details that otherwise would be difficult to detect or appreciate.Contrast agents are primarily used in the radiological or in the nuclear magnetic resonance diagnostic fields. Depending on the field of application, these derivatives present structural features, such as, in the case of molecules useful as contrast agents for X-rays analysis, the presence of one or more atom with high atomic number (e.g. iodine or barium). Iopamidol (N,N′-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-5-[(2S)(2- ...

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20-06-2013 дата публикации

Method of preparing ethacrynic amide derivatives and application thereof

Номер: US20130156701A1
Принадлежит: National Tsing Hua University NTHU

The present invention provides a method for preparing [ 18 F]—N-(4-fluorobutyl)ethacrynic amide which is prepared from radiofluorination and deprotection of the precursor tosylate N-Boc-N-[4-(toluenesulfonyloxy)-butyl)ethacrynic amide], obtained from ethacrynic acid via 6-step synthesis in 39% yield, in a radiochemical yield of 44%, aspecific activity of 48 GBq/μmol and radiochemical purity of 98%. The present invention further provides a composition for positron emission tomography (PET) of an animal models of a tumor liver or a liver disease, comprising [ 18 F]—N-(4-fluorobutyl)ethacrynic amide and a pharmaceutically acceptable carrier.

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27-06-2013 дата публикации

AMINE ADDUCTS, DERIVATIVES THEREOF, METHODS FOR MAKING SUCH ADDUCTS AND DERIVATIVES, AND METHODS FOR USING SUCH ADDUCTS AND DERIVATIVES

Номер: US20130161014A1
Принадлежит: Rhodia Operations

An amine adduct is made by (1) forming an addition intermediate by heating a mixture comprising at least one diene and at least one unsaturated fatty acyl compound, and reacting the addition intermediate with a diamine to form the amine adduct, or by (2) reacting at least one unsaturated fatty acyl compound with at least one diamine to form an amine intermediate, and heating a mixture of the amidoamine intermediate and at least one diene to form the amine adduct, or by (3) reacting at least one unsaturated fatty tertiary amine compound with at least at least one diene to form the amine adduct. A surfactant composition is derived from the amine adduct and is particularly useful in a method for enhancing the recovery of oil from a reservoir having a production wellbore, comprising introducing an aqueous flooding fluid into the reservoir at one or more locations different from the location of the production wellbore, said fluid comprising the surfactant composition and recovering the oil through the production wellbore. 1. An amine adduct , comprising the product obtained by: '(b) reacting the addition intermediate with a diamine to form the amine adduct, or', '(1)(a) forming an addition intermediate by heating a mixture comprising at least one diene and at least one unsaturated fatty acyl compound, and'} '(b) heating a mixture of the amidoamine intermediate and at least one diene to form the amine adduct, or', '(2)(a) reacting at least one unsaturated fatty acyl compound with at least one diamine to form an amidoamine intermediate, and'}(3) reacting at least one unsaturated fatty tertiary amine compound with at least at least one diene to form the amine adduct.2. The amine adduct of wherein the adduct is an amidoamine product claim 1 , obtained by: '(b) reacting the addition intermediate with a diamine to form the amidoamine product, or', '(1)(a) forming an addition intermediate by heating a mixture comprising at least one diene and at least one unsaturated fatty acyl ...

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27-06-2013 дата публикации

Process for the Preparation of Nateglinide

Номер: US20130165686A1
Принадлежит: CIPLA LIMITED

The present invention relates to a process for the preparation of substantially pure nateglinide of formula (I), substantially free from the cis-isomer and L-enantiomer and preparation of enantiomerically pure nateglinide form B, directly from the hydrolysis of a (−)-N-(trans-4-isopropylcyclohexyl-1-carbonyl)-D-phenylalanine alkyl ester in a ketonic solvent or water or mixture thereof. 2. The process according to claim 1 , wherein Alk is methyl.3. The process according to claim 1 , wherein the hydrolysis is carried out at. a temperature ranging from 0° C. to 30° C.4. The process according claim 1 , wherein the solvent is a mixture of a ketone and water claim 1 , and the ketone:water ratio varies from 5:1 to 1:1.5. The process according to . wherein the solvent comprises acetone and water.6. The process according to claim 1 , wherein the solvent is a 1:1 v/v mixture of acetone and water claim 1 , isolation of the nateglinide comprises drying under vacuum tray driers at a temperature ranging from 70° C. to 90° C. claim 1 , and the nateglinide i.s isolated in polymorphic Form B.8. The process according to claim 8 , wherein the compound (IV) is in the form of an HCl addition salt.9. The process according to claim 7 , wherein the trans-4-isopropyl-cyclobexylcarboxylic acid of formula (III) is in molar excess relative to the compound (IV).10. The process according to claim 7 , wherein the condensing reagent is selected from the group consisting of phenylsilane claim 7 , 1 claim 7 ,1′-carbonyldiimidazole (CDI) claim 7 , benzotriazol-1-yloxytris (dimethylamino) phophonium hexafluorophosphate (BOP) claim 7 , 1-hydroxy benzotriazole hydrate (HOBO claim 7 , PyBOP (Analog of the BOP) claim 7 , 1 claim 7 ,3-dicyclohexylcarbodiimide (DCC) claim 7 , 1 claim 7 ,3-chisopropylcarbodiimide (DIC) claim 7 , N claim 7 ,N-diisopropylethylamine (DIEA) claim 7 , 4-dimethylaminopyridine (DMAP) claim 7 , 1 claim 7 ,4-dithio-L-threitol (DTT) claim 7 , N-ethyl-V-(3-dimethylaminopropyl) ...

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04-07-2013 дата публикации

Cysteine protease inhibitors

Номер: US20130172232A1
Принадлежит: Medivir UK Ltd

Compounds of the formula I wherein R 2a and R 2b are independently H, halo, C 1 -C 4 alkyl, C 1 -C 4 haloalkyl or C 1 -C 4 alkoxy, or R 2a and R 2b together with the carbon atom to which they are attached form a C 3 -C 6 cycloalkyl; R 3 is a C 5 -C 10 alkyl, optionally substituted with 1-3 substituents independently selected from halo, C 1 -C 4 haloalkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkoxy; or R 3 is a C 2 -C 4 alkyl chain with at least 2 chloro or 3 fluoro substituents; or R 3 is C 3 -C 7 cycloalkylmethyl, optionally substituted with 1-3 substituents independently selected from C 1 -C 4 alkyl, halo, C 1 -C 4 haloalkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkoxy; R 4 is C 1 -C 6 alkyl, C 1 -C 6 haloalkyl, C 1 -C 6 alkoxy, C 1 -C 6 haloalkoxy, C 1 -C 6 alkylamino, C 1 -C 6 dialkylamino or; R 4 is Het or Carbocyclyl, either of which is optionally substituted with 1-3 substituents R 4 is Het, carbocyclyl, C 1 -C 6 alkyl, C 1 -C 6 haloalkyl, C 1 -C 6 alkoxy or C 1 -C 6 haloalkoxy; n is 1, 2 or 3; for the use in the prophylaxis or treatment of a disorder characterised by inappropriate expression or activation of cathepsin S.

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04-07-2013 дата публикации

PROCESSES FOR MAKING CYCLOPROPYL AMIDE DERIVATIVES AND INTERMEDIATES ASSOCIATED THEREWITH

Номер: US20130172560A1
Автор: Stranne Robert
Принадлежит: AstraZeneca AB

Presented herein are processes for making cyclopropyl amide derivatives of formula I, and/or pharmaceutically acceptable salts thereof, and intermediates associated therewith. At least one cyclopropyl amide derivative of formula I, or pharmaceutically acceptable salt thereof is useful to treat at least one histamine H3 receptor associated condition. 3. The process of claim 2 , wherein said base is sodium hydroxide.4. The process of claim 2 , wherein said peroxide is hydrogen peroxide.5. The process of claim 2 , wherein said acidic solution is an aqueous solution of sodium hydrogen sulfate.7. The process of claim 6 , wherein X is Br.8. The process of claim 6 , wherein said metal is zinc.9. The process of claim 6 , wherein said metal cyanide is zinc-(II)-cyanide.10. The process of claim 6 , wherein said catalyst is bis(tri-t-butylphosphine)palladium(0).15. The process of claim 14 , wherein said activating agent is 1 claim 14 ,1′-carbonyldiimidazole.19. The process of claim 18 , wherein the activating agent is a mixture of 1-hydroxybenzotriazole and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride.21. The process of claim 16 , wherein said acid is hydrochloric acid.23. The process of claim 17 , wherein said reducing agent is sodium triacetoxy borohydride. Presented herein are processes for making cyclopropyl amide derivatives of formula I, and/or pharmaceutically acceptable salts thereof, and intermediates associated therewith. At least one cyclopropyl amide derivative of formula I, or pharmaceutically acceptable salt thereof is useful to treat at least one histamine H3 receptor associated condition.The histamine H3 receptor is of current interest in developing new medicaments. The H3 receptor is a presynaptic autoreceptor located both in the central and peripheral nervous systems, the skin, and in organs, such as, for example, the lung, the intestine, probably the spleen, and the gastrointestinal tract. Recent evidence suggests the H3 receptor has intrinsic ...

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04-07-2013 дата публикации

Process for Manufacture of N-acylbiphenyl alanine

Номер: US20130172572A1
Принадлежит:

A novel process, novel process steps and novel intermediates useful in the synthesis of pharmaceutically active compounds, in particular neutral endopeptidase (NEP) inhibitors. 2. The process according to claim 1 , wherein the alkaline conditions comprise the use of a base selected from triethylamine claim 1 , pyridine claim 1 , N-methylpyrrole claim 1 , N-methylmorpholine claim 1 , sodium bicarbonate claim 1 , sodium carbonate claim 1 , potassium bicarbonate claim 1 , potassium carbonate claim 1 , sodium acetate claim 1 , potassium acetate claim 1 , sodium propionate and potassium propionate.3. The process according to ems claim 1 , wherein the reaction is carried out at a temperature of from of from 80 deg C. to reflux.5. The process according to claim 4 , wherein the reaction is carried out at a temperature of from of from room temperature to reflux.7. The process according to claim 6 , wherein the hydrogenation conditions comprise the use of hydrogen and palladium claim 6 , preferably claim 6 , palladium on charcoal.8. A process for preparing a compound of formula (3) claim 6 , as defined in claim 6 ,comprising the steps of{'claim-ref': [{'@idref': 'CLM-00001', 'claim 1'}, {'@idref': 'CLM-00001', 'claim 1'}], 'i) preparing the compound of formula (1-a), as defined in , according to the process defined in ;'}{'claim-ref': [{'@idref': 'CLM-00004', 'claim 4'}, {'@idref': 'CLM-00004', 'claim 4'}], 'ii) preparing the compound of formula (2-a), as defined in , according to the process defined in ; and'}{'claim-ref': {'@idref': 'CLM-00006', 'claim 6'}, 'iii) obtaining the compound of formula (3), according to the process defined in .'}9. A process for preparing a compound of formula (3) claim 6 , as defined in claim 6 ,comprising the steps of{'claim-ref': [{'@idref': 'CLM-00004', 'claim 4'}, {'@idref': 'CLM-00004', 'claim 4'}], 'ii) preparing the compound of formula (2-a), as defined in , according to the process defined in ; and'}{'claim-ref': {'@idref': 'CLM-00006', ...

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04-07-2013 дата публикации

Novel Polymers

Номер: US20130172600A1
Принадлежит: NOVARTIS AG

The invention relates to novel crosslinkable copolymers which are obtainable by (a) copolymerizing at least two different hydrophilic monomers selected from the group consisting of N,N-dimethyl acrylamide (DMA), 2-hydroxyethyl acrylate (HEA), glycidyl methacrylate (GMA), N-vinylpyrrolidone (NVP), acrylic acid (AA) and a C-C-alkoxy polyethylene glycol(meth)acrylate having a weight average molecular weight of from 200 to 1500, and at least one crosslinker comprising two or more ethylenically unsaturated double bonds in the presence of a chain transfer agent having a functional group; and (b) reacting one or more functional groups of the resulting copolymer with an organic compound having an ethylenically unsaturated group. 124-. (canceled)25. A process for manufacturing an actinically crosslinkable prepolymer , comprising:(1) obtaining a reaction mixture comprising a first hydrophilic monomer, at least one polysiloxane-containing crosslinker, a second hydrophilic monomer, and a chain transfer agent having a first functional group and present in an amount to have a desired initial concentration;(2) adjusting the temperature of the reaction mixture in order to start the polymerization reaction;(3) dosing the chain transfer agent to the reaction mixture at a rate sufficient to have a concentration comparable to the desired initial concentration until a desired total amount of the chain transfer agent is added;(4) following the completion of the chain transfer agent dosing maintaining the reaction mixture at the reaction temperature in order to complete the reaction so as to obtain a copolymerization product with first functional groups; and(5) reacting an organic compound with the copolymerization product to form the crosslinkable prepolymer having ethylenically unsaturated groups, wherein the organic compound comprises an ethylenically unsaturated group and a second functional group, wherein the second functional group of the organic compound reacts with one of the ...

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18-07-2013 дата публикации

ACID ADDITION SALT OF A NORTRIPTYLINE-GABA CONJUGATE AND A PROCESS OF PREPARING SAME

Номер: US20130184347A1
Принадлежит:

An acid addition salt of a nortriptyline-GABA conjugate, a novel crystalline form of a fumaric acid addition salt of a nortriptyline-GABA conjugate, and processes of preparing the forgoing are disclosed. Uses of the above-indicated forms of a nortriptyline-GABA conjugate in the treatment of CNS disorders, and in the treatment of pain in particular, are also disclosed. Further disclosed in a large-scale process of preparing a nortriptyline-GABA conjugate. 149-. (canceled)50. A fumaric acid addition salt of nortriptyline-4-aminobutyrate.51. A crystalline form of a fumaric acid addition salt of nortriptyline-4-aminobutyrate , characterized by at least one of:{'figref': {'@idref': 'DRAWINGS', 'FIG. 3'}, '(a) an X-Ray Powder Diffraction (XRPD) pattern exhibiting at least four of the peaks shown in ;'}{'figref': {'@idref': 'DRAWINGS', 'FIG. 1'}, '(b) an infrared spectrum exhibiting at least three of the absorption peaks shown in ; and'}(c) a Differential Scanning calorimetry (DSC) exhibiting an endothermic peak maximum that ranges from 155° C. to 160° C.52. The crystalline form of nortriptyline-4-aminobutyrate fumarate of claim 51 , characterized by an X-Ray Powder Diffraction (XRPD) pattern exhibiting at least six of the peaks shown in .53. The crystalline form of nortriptyline-4-aminobutyrate fumarate of claim 51 , characterized by an X-Ray Powder Diffraction (XRPD) pattern exhibiting at least seven of the peaks shown in .54. The crystalline form of nortriptyline-4-aminobutyrate fumarate of claim 51 , characterized by an X-Ray Powder Diffraction (XRPD) pattern substantially identical to the XRPD pattern shown in .55. The crystalline form of nortriptyline-4-aminobutyrate fumarate of claim 51 , characterized by an infrared spectrum exhibiting at least five of the absorption peaks shown in .56. The crystalline form of a fumaric acid addition salt of nortriptyline-4-aminobutyrate of claim 51 , characterized by an infrared spectrum exhibiting absorption peaks substantially ...

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18-07-2013 дата публикации

PROCESS FOR PREPARATION OF 4-FLUORO-alpha-[2METHYL-L-OXOPROPYL]-gamma-OXO-N-beta-DIPHENYLBENZENE BUTANE AMIDE

Номер: US20130184493A1
Принадлежит: VIJAYASRI ORGANICS LIMITED

A process for preparation of 4-fluoro-α-[2-methyl-1-oxopropyl]-γ-oxo-N-β-diphenylbenzene butane amide also known as a diketone intermediate of atorvastatin, completely devoid of impurities 3,4-difluoro-α-[2-methyl-1-oxopropyl]-γ-oxo-n-β-diphenylbenzene butane amide; methyl, 2{-2[-(4-fluorophenyl)-2-oxo-1-phenylethyl)]}-4-methyl-3-oxo pentanoate; 1,4-bis(4-fluorophenyl)-2,3-diphenylbutane-1,4-dione, 1-(4-fluorophenyl)-2-phenyl ethanone; 1-(4-fluorophenyl)-2-phenyl ethanone and containing about 0.05% or less of 2-methyl-1-oxopropyl]-γ-oxo-N-β-diphenylbenzene butane amide. In that process the said diketone intermediate of formula 1 is obtained by maintaining temperature −25° C. to 50° C. during Friedel-Crafts acylation, in situ halogenation of formula II in presence of a solvent and nucleophilic substitution from a compound of formula III with formula IV in presence of a base. 2. The process of claim 1 , wherein said Friedel-Crafts condensation is carried out in presence of Lewis acid catalyst to afford said Formula II.3. The process of claim 2 , wherein said lewis acid catalyst is selected from the group comprising FeCl3 claim 2 , SbCl5 claim 2 , BF3 claim 2 , TiCl4 claim 2 , ZnC2 or AlCl3.4. (canceled)5. The process of claim 1 , wherein the inert solvent in step (b) is methylene chloride.6. The process of claim 1 , wherein said halogen is selected from the group consisting of bromine and chlorine.7. The process of claim 1 , wherein said base for nucleophilic substitution of said formula III is eitherone or more inorganic salts selected from the group comprising sodium carbonate, potassium carbonate or cesium carbonate; orone or more organic bases selected from the group comprising triethyl amine or diisopropylethylamine.8. The process of claim 1 , wherein said solvent for nucleophilic substitution of said formula III is selected from the group comprising tetrahydrofuran claim 1 , 1 claim 1 ,2-dimethoxy ethane claim 1 , methylene chloride claim 1 , ethyl acetate claim ...

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25-07-2013 дата публикации

Process for the preparation of amino acid derivatives

Номер: US20130190533A1
Принадлежит: UCB PHARMA GMBH

The present invention relates to a process of manufacture of compounds of formula (B) wherein R 1 , R 2 and R 3 are as defined for compounds of formula (A), which process comprises hydrogenation of compounds of general formula (A). In particular, the present invention relates to an improved process for the manufacture of Lacosamide (LCM), (R)-2-acetamido-N-benzyl-3-methoxypropion-amide (B1), which is useful as an anticonvulsive drug.

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08-08-2013 дата публикации

PROCESSES FOR REDUCING IMPURITIES IN LACOSAMIDE

Номер: US20130204042A1
Принадлежит: RANBAXY LABORATORIES LIMITED

The present invention relates to processes for reducing impurities in lacosamide during the preparation of lacosamide. The invention provides processes for minimizing or removing impurities such as (2R)-2-(acetylamino)-3-(benzylamino)-3-oxopropyl acetate of Formula II or (2R)-2-propanoylamino-N-benzyl-3-methoxypropionamide of Formula III in lacosamide. 2. The process of wherein the lacosamide prepared is substantially free of Impurity-A and/or Impurity-B.4. The process of wherein the lacosamide prepared is substantially free of Impurity-A and/or Impurity-B.5. A process for reducing the content of “Impurity-A” in lacosamide during the preparation of lacosamide that comprises the step of treating D-serine with a protecting reagent wherein the number of moles of the protecting reagent is less than the number of moles of D-serine.6. The process of wherein the lacosamide prepared is substantially free of Impurity-A.8. The process of wherein lacosamide prepared is substantially free of Impurity-B.9. Lacosamide substantially free of Impurity-A and Impurity-B.10. Lacosamide substantially free of Impurity-A.11. Lacosamide substantially free of Impurity-B. The present invention relates to processes for reducing impurities in lacosamide during preparation of lacosamide. The invention provides processes for minimizing or removing impurities such as (2R)-2-(acetylamino)-3-(benzylamino)-3-oxopropyl acetate of Formula II or (2R)-2-propanoylamino-N-benzyl-3-methoxypropionamide of Formula III in lacosamide.Lacosamide (SPM 927, also referred to as harkoseride or ADD 234037), is chemically (R)-2-acetamido-N-benzyl-3-methoxypropionamide and represented by Formula I. It has been reported to be effective for the treatment of pain, epilepsy, fibromyalgia syndrome, osteoarthritis and migraine. It is also known to be useful for the treatment of CNS disorders in humans.Lacosamide is available in the United States market as solution and tablet dosage forms with proprietary name of Vimpat®. ...

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15-08-2013 дата публикации

Process for the Preparation of Prostaglandin Analogues

Номер: US20130211128A1
Принадлежит: SCINOPHARM TAIWAN LTD.

A process for preparing a prostaglandin analogue comprising a step of converting a compound of formula (8′): 2. The process of wherein the compound of formula (11) is travoprost.3. The process of wherein the compound of formula (11) is bimatoprost.5. The process of wherein the step (b) comprising steps of:(1) reducing the ketone group of compound of formula (10B);(2) deprotecting the reduced form of the compound of formula (10B); and(3) reacting the resultant compound of step (2) with ethylamine to give the bimatoprost.6. The process of wherein the step (3) is conducted in the presence of 40 to 80% v/v ethylamine in methanol.7. The process of wherein the step (b) comprising steps of:(1) reducing the ketone group of compound of formula (10B);(2) reacting the reduced compound of step (1) with ethylamine; and(3) deprotecting the resultant compound of step (2) to give the bimatoprost.8. The process of wherein the step (2) is conducted in the presence of 40 to 80% v/v ethylamine in methanol. This application is a divisional of U.S. patent application Ser. No. 12/905,439 which was filed with the U.S. Patent and Trademark Office on Oct. 15, 2010, which is a divisional of U.S. patent application Ser. No. 12/421,185 which was filed with the U.S. Patent and Trademark Office on Apr. 9, 2009, which claims priority from U.S. Provisional Patent Application Ser. No. 61/123,527 which was filed on Apr. 9, 2008. The entire content of these related applications is explicitly incorporated herein as reference.1. Field of the InventionThe present application is directed to intermediates for preparing prostaglandin analogues and processes for preparing prostaglandin analogues and intermediates thereof.2. Description of the Related ArtNatural prostaglandins have a unique structure based on prostanoic acid and exhibit a broad range of physiological activities even when present in extremely small amounts, attracting interest of many organic synthetic chemists. Therefore, various processes to ...

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22-08-2013 дата публикации

SYNTHESIS OF CYCLOHEXANE DERIVATIVES USEFUL AS SENSATES IN CONSUMER PRODUCTS

Номер: US20130216486A1
Принадлежит: The Procter & Gamble Company

The present invention provides synthetic routes for preparing various isomers of cyclohexane-based coolants, such as menthyl esters and menthanecarboxamide derivatives, in particular those substituted at the amide nitrogen, for example with an aromatic ring or aryl moiety. Such structures have high cooling potency and long lasting sensory effect, which make them useful in a wide variety of consumer products. One synthetic route involves a copper catalyzed coupling of a primary menthanecarboxamide with an aryl halide, such reaction working best in the presence of potassium phosphate and water. Using this synthetic route, specific isomers can be prepared including the menthanecarboxamide isomer having the same configuration as l-menthol and new isomers such as a neoisomer having opposite stereochemistry at the carboxamide (C-1) position. The neoisomer unexpectedly has potent and long lasting cooling effect. Preparation schemes for neoisomers of other menthyl derivatives which are useful as coolants, including esters, ethers, carboxy esters and other N-substituted carboxamides are also provided. 2. The process of wherein the reaction is conducted in the presence of potassium phosphate and the copper catalyst is a copper halide.3. The process of wherein the copper halide is copper (I) iodide.4. The process of wherein the primary menthane carboxamide is prepared by reacting a menthane acid chloride with ammonia under aqueous conditions.5. The process of wherein the menthane carboxamide is prepared by hydrolysis of a corresponding menthane nitrile.6. The process of wherein the stereochemistry of the starting menthane carboxamide is maintained through the coupling reaction with aryl halide to produce the N-substituted menthane carboxamide.7. The process of wherein (1S claim 6 ,2S claim 6 ,5R)-menthane carboxamide is reacted with aryl halide to produce neoisomers having 1S claim 6 ,2S claim 6 ,5R configuration of N-aryl substituted menthane carboxamide.8. A process for ...

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29-08-2013 дата публикации

Fluoroalkylation Methods And Reagents

Номер: US20130225815A1
Принадлежит: University of Illinois

A method of forming a fluorinated molecular entity includes reacting in a reaction mixture an aromatic halide, copper, a fluoroalkyl group, and a ligand. The aromatic halide includes an aromatic group and a halogen substituent bonded to the aromatic group. The ligand includes at least one group-V donor selected from phosphorus and an amine. The overall molar ratio of copper to aromatic halide in the reaction mixture is from 0.2 to 3. The method further includes forming a fluoroalkylarene including the aromatic group and the fluoroalkyl group bonded to the aromatic group. A composition, which may be used in the method, consists essentially of copper, the fluoroalkyl group, and the ligand, where the molar ratio of copper to the fluoroalkyl group is approximately 1.

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12-09-2013 дата публикации

Process for Preparing Esteramide Compounds

Номер: US20130237722A1
Принадлежит: Rhodia Operations

The present invention relates to a method for preparing esteramide compounds. More particularly, the invention relates to a method for preparing esteramide compounds by reaction between a diester and an amine, in the presence of a basic compound, wherein 1. A method for preparing an esteramide compound of the following formula (I):{'br': None, 'sup': 1', '2', '3, 'ROOC-A-CONRR\u2003\u2003(I)'}comprising a reaction step between: {'br': None, 'sup': 1', '1, 'ROOC-A-COOR\u2003\u2003(II)'}, 'a diester compound of the following formula (II) {'br': None, 'sup': 2', '3, 'HNRR\u2003\u2003(III)'}, 'and an amine of the following formula (III)in the presence of a basic compound, A is a covalent bond or a linear or branched divalent alkylene group comprising a number of carbon atoms ranging from 1 to 12,', {'sup': '1', 'Ris an optionally substituted hydrocarbon group, comprising from 1 to 36 carbon atoms,'}, {'sup': 2', '3, 'Rand R, either identical or different, are groups selected from hydrogen and optionally substituted hydrocarbon groups, comprising from 1 to 36 carbon atoms,'}, {'sup': 2', '3, 'Rand Rmay form together a ring comprising the nitrogen atom to which they are bound, said ring being substituted, if necessary, and/or comprising an additional heteroatom, and'}, {'sup': 2', '3, 'Rand Rnot being simultaneously hydrogen atoms,'}], 'wherein the amine (III) is solubilized in an organic solvent, or in the diester compound (II),', 'when the amine (III) is solubilized in an organic solvent, the diester compound (II) is added onto the reaction mixture comprising the amine (III) and the basic compound,', 'when the amine (III) is solubilized in the diester compound (II), the basic compound is added onto the reaction mixture comprising the amine (III) and the diester compound (II),', 'the reaction is conducted at a temperature greater than or equal to 30° C.,', 'the amine (III) is present in molar excess ranging from 0.01 to 50%, based on the diester compound (II)., ' ...

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19-09-2013 дата публикации

Compound having hetero ring skeleton, and process for producing optically active compound using the aforementioned compound as asymmetric catalyst

Номер: US20130245257A1
Принадлежит: KYOTO UNIVERSITY, Sumitomo Chemical Co Ltd

The invention provides a compound having a heterocyclic skeleton of formula (I): wherein the substituents are as defined in the specification, as well as a tautomer thereof or a salt thereof. The invention also provides asymmetric synthesis methods involving the use of such a compound, tautomer thereof, or salt thereof, as a catalyst.

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19-09-2013 дата публикации

Synthesis of Trivalent Flexible Frameworks with Ligands Comprising Catechol Units for Functionalizing Surfaces

Номер: US20130245270A1
Принадлежит: JUSTUS-LIEBIG-UNIVERSITAT GIESSEN

The present invention describes tripodal catechol derivatives with a flexible basic framework for the functionalisation of surfaces, and methods for their production and use. The central atom of the flexible framework is hereby a tertiary aliphatic carbon atom. The remaining fourth bridgehead position is easily suitable to be further functionalised via so-called click reactions, e.g. with biomolecules, dyes, radiomarkers, polyethylene glycol or active agents. 2. The compound according to claim 1 , wherein Y is a bond claim 1 , —CH— claim 1 , —NH—(C═O)— claim 1 , —(C═O)—NH— claim 1 , or —NR—.3. The compound according to claim 1 , wherein n is an integer between 0 and 3.4. The compound according to claim 1 , m is an integer between 0 and 3.7. The compound according to claim 1 , wherein X is —(CH)—R claim 1 , and p is an integer between 0 and 3.8. The compound according to claim 1 , wherein{'sub': 2', 'p, 'sup': '5', 'X is —(CH)—R,'}{'sup': 5', '6', '6', '7', '6, 'sub': 2', '2', '2', '2, 'Ris —H, —OH, —NH, —NO, —NH—NH, —NHR, —NRR, —O—NH, —NH—(C═O)—C≡CH, —C≡CH, —N═C═S, —N═C═O, —COOH, —(C═O)H, or —(C═O)R, and'}p is an integer between 0 and 3.10. The method according to claim 9 , wherein X is a hydrogen atom.11. The method according to claim 9 , wherein{'sub': 2', 'p, 'sup': '5', 'X is —(CH)—R,'}{'sup': 5', '6', '6', '7', '6, 'sub': 2', '2', '2', '2, 'Ris —OH, —NH, —NO, —NH—NH, —NHR, —NRR, —O—NH, —NH—(C═O)—C≡CH, —C≡CH, —N═C═S, —N═C═O, —COOH, —(C═O)H, or —(C═O)R, and'}p is an integer between 0 and 3.12. The method according to claim 11 , wherein Ris protected by a protective group (Pg) prior to reacting the compound with the reagent Y″Z claim 11 , so that the compound Pg-X—C[(CH)—Y′]is reacted with the reagent Y″Z to produce a corresponding compound Pg-X—C[(CH)—YZ].13. (canceled)14. (canceled)15. (canceled) The present invention describes tripodal catechol derivatives with a flexible basic framework for the functionalisation of surfaces, and methods for their production ...

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19-09-2013 дата публикации

METHOD FOR PRODUCING SANSHOOL

Номер: US20130245303A1
Автор: Aoki Katsuyuki
Принадлежит: TSUMURA & CO.

Provided are a method for producing a sanshool, which method has a short process and exhibits high stereoselectivity, as well as an iron carbonyl complex compound that is an intermediate useful for the production method. 4. The method for producing a sanshool according to claim 3 , wherein the deprotecting agent is one selected from the group consisting of cerium (IV) compounds claim 3 , trimethylamine N-oxide claim 3 , pyridine N-oxide claim 3 , iron (III) chloride claim 3 , copper (II) chloride claim 3 , dichlorodicyano benzoquinone claim 3 , and hydrogen peroxide. The present invention relates to a method for producing a sanshool and to a diene iron complex compound that is an intermediate useful for the production method. In particular, the invention relates to a method for producing a sanshool, which can produce a sanshool in a short process and with high stereoselectivity, as well as to a novel diene iron complex compound that is an intermediate useful for the production method.Sanshools are a main ingredient of a crude drug, “Zanthoxylum Fruit”. In recent years, HαS (hydroxy-α-sanshool) has been reported to have effects such as stimulations of TRPV1 and TRPA1 and is now in the spotlight of the medicinal chemical field.Sanshools including HαS have an unstable structure due to a triene moiety. Therefore, it has been difficult to constantly produce and supply sanshool as a pure substance. Conventionally, sanshools have been isolated and purified from an extract of sanshoo as a raw material by silica gel and ODS column chromatography.Total syntheses of HαS and HβS (hydroxy-β-sanshool) have not been reported in the past, but a total synthesis of α-sanshool as an analogue thereof has been reported (see Non-Patent Documents 1 and 2). Methods described in the Non-Patent Documents 1 and 2 are both those for forming a triene moiety by a Wittig reaction.However, the methods described in Non-Patent Documents 1 and 2 have showed low yield and low E/Z selectivity and thus ...

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03-10-2013 дата публикации

PHENOXYPROPANOL DERIVATIVES AND THEIR USE IN TREATING CARDIAC AND CARDIOVASCULAR DISEASES

Номер: US20130261178A1
Принадлежит:

A compound of formula I-0, and its pharmaceutically acceptable salt or salts and physiologically hydrolysable derivatives in free form or salt form: 2. The compound as claimed in wherein Ris selected from unsubstituted and substituted Ccycloalkyl claim 1 , Ccycloalkyl-Calkyl claim 1 , Calkyl claim 1 , Caryl-Calkyl claim 1 , Calkoxy-Caryl-Calkyl.3. The compound as claimed in wherein Xis selected from CO claim 1 , CS claim 1 , SOand a single bond.4. The compound as claimed in wherein Rand Rare selected from ROZO as hereinbefore defined claim 1 , m- claim 1 ,p-(OCH)or o- claim 1 , m- or p-OH claim 1 , F claim 1 , Cl claim 1 , Br claim 1 , NH claim 1 , R claim 1 , OR claim 1 , or CFor a combination thereof.12. A process for the preparation of a compound of formula I-0 or subformulae as defined in .14. A composition comprising a therapeutically effective amount of a compound of formula I-0 or subformulae or its pharmaceutically acceptable salt and physiologically hydrolysable derivative as defined in in association with one or more pharmaceutical carriers or diluents.15. The use of a compound of formula I-0 or subformulae or pharmaceutically acceptable salt or composition as defined in in the prevention or treatment of a condition selected from ischaemic heart disease claim 1 , hypertension and heart failure claim 1 , more preferably with concomitant respiratory disease claim 1 , in particular asthma or COPD.16. A method of treating a condition selected from ischaemic heart disease (also known as myocardial infarction or angina) claim 1 , hypertension and heart failure claim 1 , restenosis and cardiomyopathy claim 1 , more preferably with concomitant respiratory disease claim 1 , in particular asthma or COPD claim 1 , said method comprising administering to a subject in need thereof claim 1 , a compound of formula I-0 or subformulae or pharmaceutically acceptable salt or composition thereof as defined in in an amount sufficient to treat the condition.17. A method of ...

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03-10-2013 дата публикации

GENETICALLY ENCODED INITIATOR FOR POLYMER GROWTH FROM PROTEINS

Номер: US20130261259A1
Принадлежит: FRANKLIN AND MARSHALL COLLEGE

This invention pertains to methods for producing homogeneous recombinant proteins that contain polymer initiators at defined sites. The unnatural amino acid, 4-(2′-bromoisobutyramido)phenylalanine of formula 1, was designed and synthesized as a molecule comprising a functional group further comprising an initiator for an atom-transfer radical polymerization (‘ATRP”) that additionally would provide a stable linkage between the protein and growing polymer. We evolved a (Mj) tyrosyl-tRNA synthetase/tRNApair to genetically encode this unnatural amino acid in response to an amber codon. To demonstrate the utility of this functional amino acid, we produced Green Fluorescent Protein with the unnatural amino acid initiator of formula 1 site-specifically incorporated on its surface (GFP-1). Purified GFP-1 was then used as an initiator under standard ATRP conditions with oligo(ethylene oxide)monomethyl ether methacrylate, efficiently producing a polymer-GFP bioconjugate wherein the polymer is connected at a specifically selected site on GFP. 2. The compound of claim 1 , as described by formula 6 claim 1 , wherein R1 and R2 are independently H claim 1 , methyl claim 1 , or phenyl; X is F claim 1 , Cl claim 1 , Br claim 1 , I; or N; A is O claim 1 , S claim 1 , or NR claim 1 , wherein R is H claim 1 , methyl claim 1 , or phenyl; n is 1; or a salt thereof.6. The compound of claim 1 , wherein R1 and R2 are independently H claim 1 , methyl claim 1 , or phenyl; X is F claim 1 , Cl claim 1 , Br claim 1 , I claim 1 , or N; A is O claim 1 , S claim 1 , or NR claim 1 , wherein R is H claim 1 , methyl claim 1 , or phenyl; n is 0; or a salt thereof.14. The method of claim 13 , wherein R1 and R2 are independently H claim 13 , methyl claim 13 , or phenyl; X is F claim 13 , Cl claim 13 , Br claim 13 , I claim 13 , or N; Y is F claim 13 , Cl claim 13 , Br claim 13 , I claim 13 , or trifluoroacetate; A is O claim 13 , S claim 13 , or NR claim 13 , wherein R is H claim 13 , methyl claim 13 , ...

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03-10-2013 дата публикации

SYNTHESIS OF ALISKIREN

Номер: US20130261324A1
Принадлежит:

The present invention provides novel process for the preparation of renin inhibitor Aliskiren or its derivatives, and its pharmaceutically acceptable salts. The present invention also provides novel intermediates used in the preparation of Aliskiren. 3. The process according to claim 1 , wherein the reduction of the azide group of the compound of Formula-IV is carried out by using a palladium catalyst.4. The process according to claim 1 , wherein the reduction of the azide group of the compound of Formula-IV is carried out in the presence of an alcoholic solvent.5. The process according to claim 4 , wherein the alcoholic solvent used in the reduction of the azide compound of Formula-IV is selected from the group consisting of ethanol claim 4 , methanol claim 4 , and isopropanol.7. The process according to claim 6 , wherein the compound of Formula-V is purified by fractional distillation.9. Use of a compound of Formula-III as a starting compound in the preparation of Aliskiren or a pharmaceutically acceptable salts thereof. The present invention relates to novel process for the preparation of renin inhibitor Aliskiren or its derivatives, and its pharmaceutically acceptable salts.Aliskiren, (2S,4S,5S,7S)—N-(2-carbamoyl-2-methylpropyl)-5-amino-4-hydroxy-2,7-diisopropyl-8-[4-methoxy-3-(3-methoxypropoxy)phenyl]octanamide having the Formula-I, a new antihypertensive has been developed which interferes with the renin-angiotensin system at the beginning of angiotensin II biosynthesis.Aliskiren is marketed by Novartis as TEKTURNA® in the form of its hemifumarate salt in a once-daily formulation. More recently Aliskiren is also formulated as combination with other API.U.S. Pat. No. 5,559,111 discloses Aliskiren and related compounds along with the different approaches for the synthesis of Aliskiren.Further U.S. Pat. No. 7,132,569, U.S. Pat. No. 7,009,078, U.S. Pat. No. 6,730,798 and U.S. Pat. No. 6,800,769 claims novel intermediates used in the preparation of Aliskiren and ...

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03-10-2013 дата публикации

METHOD FOR PRODUCING SANSHOOL

Номер: US20130261327A1
Автор: Aoki Katsuyuki
Принадлежит: TSUMURA & CO.

Provided are a method for producing a sanshool, which can produce a sanshool in a short process and with high stereoselectivity, as well as a novel diene iron complex compound that is a stable intermediate useful for the production method. The diene iron complex compound is represented by the following general formula (I): 3. The method for producing a sanshool according to claim 2 , wherein the deprotecting agent is selected from the group consisting of cerium (IV) compounds claim 2 , trimethylamine N-oxide claim 2 , pyridine N-oxide claim 2 , iron (III) chloride claim 2 , copper (II) chloride claim 2 , dichlorodicyano benzoquinone claim 2 , and hydrogen peroxide.5. The method for producing a sanshool according to claim 4 , wherein lithium hydroxide is used as a base in the step of reacting the aldehyde compound with (E)-N-isobutyl-diethylphosphonocrotonic acid amide claim 4 , (E)-N-(2-methyl-2-hydroxy-propyl)-diethylphosphonocrotonic acid amide claim 4 , or (E)-N-(2 claim 4 ,2-dimethyl-propyl)-diethylphosphonocrotonic acid amide.7. The method for producing a sanshool according to claim 6 , wherein lithium hydroxide is used as a base in the step of reacting the aldehyde compound with triethyl 4-phosphonocrotonate.9. The method for producing a sanshool according to claim 8 , wherein lithium hydroxide is used as a base in the step of reacting the aldehyde compound with triethyl 4-phosphonocrotonate. The present invention relates to a method for producing a sanshool and to a diene iron complex compound that is an intermediate useful for the production method. In particular, the invention relates to a method for producing a sanshool, which can produce a sanshool in a short process and with high stereoselectivity, as well as to a novel diene iron complex compound that is an intermediate useful for the production method.Sanshools are a main ingredient of a crude drug, “Zanthoxylum Fruit”. In recent years, gamma-sanshool has been reported to have effects such as the ...

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10-10-2013 дата публикации

Aromatic ketone synthesis with amide reagents and related reactions

Номер: US20130267712A1
Принадлежит: Northern Illinois University

A method of preparing an aryl carbonyl or aryl thiocarbonyl compound, comprises reacting an N-(nitroaryl)-amide or N-(nitroaryl)-thioamide with an aromatic ring, with a superacid catalyst, to produce the aryl carbonyl or aryl thiocarbonyl compound. The superacid is present in an amount of at most 8 equivalents in proportion to the N-(nitroaryl)-amide or N-(nitroaryl)-thioamide. A method of preparing aryl amide or aryl thioamide, comprises reacting an N-(nitroaryl)-carbamide or N-(nitroaryl)-thiocarbamide with an aromatic ring, with a superacid catalyst, to produce the aryl amide or aryl thioamide.

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10-10-2013 дата публикации

BIDENTATE CHIRAL LIGANDS FOR USE IN CATALYTIC ASYMMETRIC ADDITION REACTIONS

Номер: US20130267714A1
Принадлежит:

Compounds of the formula (I) in the form of a mixture of predominantly one diastereomer or in the form of pure diastereomers, 1. Compounds of the formula (I) in the form of a mixture of predominantly one diastereomer or in the form of pure diastereomers ,{'br': None, 'sub': 1', '0', '1, 'Z-Q-P*RR\u2003\u2003(I),'}wherein:{'sub': 1', '2, 'claim-text': {'sub': 1', '6', '1', '6', '1', '4', '2', '6', '5', '3', '1', '12', '3, 'wherein R is a hydrocarbon radical or O-atom(s)-containing heterohydrocarbon radical having 1 to 18 carbon atoms and optionally substituted by C-C-alkyl, trifluoromethyl, C-C-alkoxy, trifluoromethoxy, (C-C-alkyl)amino, (CH)Si, (C-C-alkyl)Si or halogen;'}, 'Zis a C-bonded, secondary phosphine group of the formula —P(R),'} [{'sub': 1', '0', '1, '(i) an optionally substituted achiral aromatic group, wherein the achiral aromatic group is bonded directly to Zthrough a carbon atom of the achiral aromatic group and bonded directly to P*RRthrough a carbon atom of the achiral aromatic group, and'}, {'sub': 1', '4, '(ii) an optionally substituted C-C-alkylene group;'}], 'Q is selected from the group consisting ofP* is a chiral phosphorus atom;{'sub': '0', 'Ris methyl; and'}{'sub': '1', 'Ris a C-bonded optically enriched or optically pure chiral, mono- or polycyclic, nonaromatic hydrocarbon ring.'}23-. (canceled)4. The compounds according to claim 1 , wherein the secondary phosphine Zis selected from the group consisting of: —P(C-C-alkyl) claim 1 , —P(C-C-cycloalkyl) claim 1 , —P(o-furyl) claim 1 , —P(CH) claim 1 , —P[2-(C-C-alkyl)CH] claim 1 , —P[3-(C-C-alkyl)CH] claim 1 , —P[4-(C-C-alkyl)CH] claim 1 , —P[2-(C-C-alkoxy)CH] claim 1 , —P[3-(C-C-alkoxy)CH] claim 1 , —P[4-(C-C-alkoxy)CH] claim 1 , —P[2-(trifluoromethyl)CH] claim 1 , —P[3-(trifluoromethyl)CH] claim 1 , —P[4-(trifluoromethyl)CH] claim 1 , —P[3 claim 1 ,5-bis(trifluoromethyl)CH] claim 1 , —P[3 claim 1 ,5-bis(C-C-alkyl)CH] claim 1 , —P[3 claim 1 ,5-bis(C-C-alkoxy)CH]and —P[3 claim 1 ,5-bis(C-C-alkyl ...

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17-10-2013 дата публикации

Processes For Preparing A Polymeric Compound

Номер: US20130274502A1
Принадлежит: POLYMEDIX, INC.

The present invention provides methods for preparing a polymeric compound of Formula I: The present invention was supported, in part, by funds from the U.S. Government (SBIR Phase 1 grant No. 1R43HL090113-01) and the U.S. Government may therefore have certain rights in the invention.The present invention is directed, in part, to methods for preparing a polymeric salicylamide compound and/or pharmaceutically acceptable salts thereof, as well as to useful intermediates for the preparation of the polymeric salicylamide compound and/or pharmaceutically acceptable salts thereof.The polymeric salicylamide compound of Formula I:and/or pharmaceutically acceptable salts thereof are useful, for example, as pharmaceutical agents for inhibiting angiogenesis (see, WO 2005/123660). Given the importance of the compound of Formula I and/or pharmaceutically acceptable salts thereof as pharmaceutical agents, effective synthetic methods for preparing the compound and its pharmaceutically acceptable salts is of great import. This invention is directed to this, as well as other, important ends.The present invention provides, in part, methods for preparing a compound of Formula I:or pharmaceutically acceptable salt thereof, comprising:a) removing the Cbz groups from a compound of Formula II:or pharmaceutically acceptable salt thereof, under a hydrogenation/hydrogenolysis condition to form the compound of Formula I, or pharmaceutically acceptable salt thereof; andb) optionally isolating the compound of Formula I, or pharmaceutically acceptable salt thereof.In some embodiments, the hydrogenation/hydrogenolysis condition comprises using a metal catalyst. In some embodiments, the metal catalyst is Pd/C. In some embodiments, the reaction yield in step a) is greater than about 85%.In some embodiments, the methods further comprise:c) removing the Boc group from a compound of Formula III:or pharmaceutically acceptable salt thereof, in the presence of an acid to form the compound of Formula II, ...

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24-10-2013 дата публикации

Novel ruthenium complexes and their uses in processes for formation and/or hydrogenation of esters, amides and derivatives thereof

Номер: US20130281664A1
Принадлежит: Yeda Research and Development Co Ltd

The present invention relates to novel Ruthenium catalysts and related borohydride complexes, and the use of such catalysts, inter alia, for (1) hydrogenation of amides (including polyamides) to alcohols and amines; (2) preparing amides from alcohols with amines (including the preparation of polyamides (e.g., polypeptides) by reacting dialcohols and diamines and/or by polymerization of amino alcohols); (3) hydrogenation of esters to alcohols (including hydrogenation of cyclic esters (lactones) or cyclic di-esters (di-lactones) or polyesters); (4) hydrogenation of organic carbonates (including polycarbonates) to alcohols and hydrogenation of carbamates (including polycarbamates) or urea derivatives to alcohols and amines; (5) dehydrogenative coupling of alcohols to esters; (6) hydrogenation of secondary alcohols to ketones; (7) amidation of esters (i.e., synthesis of amides from esters and amines); (8) acylation of alcohols using esters; (9) coupling of alcohols with water to form carboxylic acids; and (10) dehydrogenation of beta-amino alcohols to form pyrazines. The present invention further relates to the novel uses of certain pyridine Ruthenium catalysts.

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31-10-2013 дата публикации

PROCESS FOR THE PREPARATION OF PRAZIQUANTEL

Номер: US20130289275A1
Принадлежит:

The present disclosure describes a novel, cost-effective process for preparation of a 4-oxo-1,2,3,6,7,11b-hexahydro-4H-pyrazino-[2,1-a]isoquinoline derivatives. Specifically, it discloses a process for the preparation of the anthelmintic drug praziquantel through the use of a novel intermediate, 2-[(2,2-dimethoxyethyl)benzyl amino]-N-phenethylacetamide. This present disclosure also describes a novel crystalline form of 4-oxo-1,2,3,6,7,11b-hexahydro-4H-pyrazino[2,1-a]isoquinoline. 1. A process for the preparation of 2-[(2 ,2-dimethoxyethyl)amino]-N-(2-phenylethyl)acetamide , which comprises:a) condensation of β-phenylethylamine with chloroacetyl chloride in the presence of a solvent and a base to obtain 2-chloro-N-phenethylacetamide;b) condensation of benzylamine with chloroacetaldehyde dimethylacetal in the presence of water and a base to obtain N-benzyl-2,2-dimethoxyethanamine;c) condensation of 2-chloro-N-phenethylacetamide prepared in step a) with N-benzyl-2,2-dimethoxyethanamine of formula VI prepared in step b) in the presence of water and a base to obtain 2-[(2,2-dimethoxyethyl)benzylamino]-N-phenethylacetamide; andd) reduction of 2-[(2,2-dimethoxyethyl)benzylamino]-N-phenethylacetamide using a reducing agent and a solvent in the presence of hydrogen to obtain 2-[(2,2-dimethoxyethyl)amino]-N-(2-phenylethyl)acetamide.2. A process according to claim 1 , wherein the solvent in step a) is toluene and the base in step a) is sodium bicarbonate.3. A process according to claim 1 , wherein the solvent in step b) and step c) is water and the base in step b) and step c) is sodium hydroxide.4. A process according to claim 1 , wherein the solvent in step d) is selected from the group consisting of methanol claim 1 , ethanol claim 1 , and isopropanol claim 1 , and the reducing agent in step d) is selected from the group consisting of Raney nickel claim 1 , platinum claim 1 , and palladium on carbon.5. A process for preparation of praziquantel which comprises:{'claim-ref': ...

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31-10-2013 дата публикации

PROCESS FOR THE SYNTHESIS OF AGOMELATINE

Номер: US20130289308A1
Принадлежит: LES LABORATOIRES SERVIER

Process for the industrial synthesis of the compound of formula (I) 126-. (canceled)29. The process according to claim 27 , wherein the group Xa represents —S—C(S)—OCH.30. The process according to claim 27 , wherein the free radical reactions are initiated by thermal means at a temperature of from 50 to 140° C.31. The process according to claim 27 , wherein the step of addition of the compound of formula (II) to the compound of formula (III) is initiated in the presence of dilauroyl peroxide.32. The process according to claim 27 , wherein the reaction of cyclisation of the adduct of formula (IV) is carried out in the presence of dilauroyl peroxide optionally with dibenzoyl peroxide.33. The process according to claim 27 , wherein the step of addition of the compound of formula (II) to the compound of formula (III) and the step of cyclisation of the adduct of formula (IV) are carried out in ethyl acetate.36. The process according to claim 35 , wherein X represents Cl.37. The process according to claim 35 , wherein X represents Br.38. The process according to claim 27 , wherein the reaction deprotecting the amine function of the compound of formula (V) claim 27 , when the amine function is protected by a phthalimide group claim 27 , is carried out in the presence of sodium borohydride or a hydrazine-type agent.39. The process according to claim 34 , wherein the step of aromatisation of the compound of formula (VII) is carried out using a benzoquinone.40. The process according to claim 39 , wherein the benzoquinone is 2 claim 39 ,3-dichloro-5 claim 39 ,6-dicyano-1 claim 39 ,4-benzoquinone (DDQ).41. The process according to claim 35 , wherein the aromatisation of the compound of formula (VI) is carried out in the presence of a strong non-nucleophilic base.42. The process according to claim 35 , wherein the aromatisation of the compound of formula (VI) is carried out in the presence of an alcoholate/alcohol couple.43. The process according to claim 42 , wherein the ...

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07-11-2013 дата публикации

PROCESS FOR PRODUCING OSELTAMIVIR PHOSPHATE AND INTERMEDIATE COMPOUND

Номер: US20130296600A1
Принадлежит:

Disclosed are a process suited to large scale synthesis with high yield for producing oseltamivir phosphate, in which a preparation of oseltamivir phosphate which is highly safe as a pharmaceutical product can be produced, and an intermediate compound for producing oseltamivir phosphate. In this production process, an intermediate compound represented by general formula (V) is synthesized by employing Michael reaction/Michael reaction/Horner-Wadsworth-Emmons reaction, and oseltamivir phosphate is produced by converting the substituent groups in this intermediate compound. 39-. (canceled) The present invention relates to a process for producing oseltamivir phosphate and an intermediate compound.Influenza is an acute infectious disease caused by an influenza virus, and has been known to allow global pandemic threats to emerge every year. Influenza viruses infect host cells by incorporation of hemagglutinin that is a protein present on the surface of virus particles into host cells via binding to a glycoprotein on the surface of the host cells, followed by proliferation in the host cells, and subsequently the viruses are secreted out of the cells and infect another host cells.When thus proliferated influenza viruses in host cells are secreted out of the cells, glycoproteins present on the cell surface of the host cells form complexes with hemagglutinin present on the surface of the virus particles. For releasing the virus particles from the host cells to infect other host cells, it is necessary to cleave binding between the glycoprotein and hemagglutinin, and the cleavage of this binding is carried out by neuraminidase present on the surface of the virus particles.Oseltamivir phosphate has been known to inhibit the activity of neuraminidase, and has been used as a specific medicine for influenza. Oseltamivir phosphate has been conventionally synthesized by way of semisynthesis using shikimic acid, which is a natural substance, as a starting material (for example, see ...

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07-11-2013 дата публикации

Acetamide Stereoisomer

Номер: US20130296607A1
Принадлежит:

The compound of formula (I) 2. A process according to wherein the trialkylsilyl is TBDMS.4. A process according to wherein the trialkylsilyl is TBDMS. This application is a continuation of U.S. patent application Ser. No. 12/196,520, filed Aug. 22, 2008, now allowed. U.S. patent application Ser. No. 12/196,520 claims priority to U.S. Provisional Application No. 60/966,438 filed Aug. 28, 2007. The entire disclosures of each of these applications are hereby incorporated herein by reference.The present invention relates to a novel acetamide stereoisomer, to a process for preparing the acetamide stereoisomer, to a pharmaceutical composition comprising the acetamide stereoisomer and to the use of the acetamide stereoisomer in therapy, in particular in the treatment of bronchoconstriction associated with reversible obstructive airways diseases including but not limited to asthma, cystic fibrosis and chronic obstructive pulmonary disease, including chronic bronchitis and emphysema.Patients suffering from bronchoconstriction associated with reversible obstructive airways diseases are generally treated using a bronchodilator, to relax the bronchial smooth muscle.Bronchodilators in use today generally fall into two classes, the β-selective adrenoceptor agonists, such as albuterol (salbutamol), salmeterol and formoterol, and the muscarinic receptor antagonists, such as ipratropium and tiatropium.β-Selective adrenoceptor agonists may cause adverse effects, and these may in part be due to activation of the β-adrenoceptor. The selectivity of an agonist for the β-adrenoceptor receptor is therefore very important, because it limits the dose that can be given and so affects the magnitude of bronchodilations and the frequency of dosing.A long duration of action is important to patients, not only to minimize the time spent taking the drug, but also to avoid having to take the drug during inconvenient times, for example at work, school or during the night. Some of the more recent β- ...

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14-11-2013 дата публикации

POLYMER PRECURSORS OF RADIOLABELED COMPOUNDS, AND METHODS OF MAKING AND USING THE SAME

Номер: US20130303757A1
Принадлежит:

One aspect of the present invention relates to novel compounds that can be used to prepare radiolabeled compounds in an effective manner. A second aspect of the present invention relates to a method of synthesizing radiolabeled compounds. 115-. (canceled)16. A method for preparing a radiolabeled compound , the method comprising: reacting a polymer precursor compound with an oxidant , a radiolabeled compound and optionally a buffer , wherein the compound is selected from the group consisting of:Poly-(4S, 5S)-2-(5-{dibutyl[2-(4-vinylphenyl)ethyl]stannyl}-2,3-dihydrobenzofuran-7-yl)-3, 4-dimethyl-5-phenyl-1, 3-oxazolidine-co-divinylbenzene;Poly-5-{dibutyl[2-(4-vinylphenyl)ethyl]stannyl}-2, 3-dihydrobenzofuran-7-carbaldehyde-co-divinylbenzene;Poly-5-{dibutyl[2-(4-vinylphenyl)ethyl]stannyl}-2, 3-dihydrobenzofuran-7-carboxylic acid-co-divinylbenzene;Poly-(4S, 5S)-2-(4-{dibutyl[2-(3-vinylphenyl)ethyl]stannyl}phenyl)-3, 4-dimethyl-5-pheynyl-1, 3-oxazolidine-co-divinylbenzene; andPoly-(4S, 5S)-2-(4-{dibutyl[2-(4-vinylphenyl)ethyl]stannyl}phenyl)-3, 4-dimethyl-5-phenyl-1, 3-oxazolidine-co-divinylbenzene.17. A method of claim 16 , further comprising a purification of the radiolabeled compound.18. A kit containing a radiolabeling system claim 16 , comprising: a polymer precursor compound and instructions for using said polymer precursor compound claim 16 , wherein said polymer precursor compound comprises the polymer precursor compound of .19. The kit of that further includes a filter or a filtration device.20. The kit of that further includes a chelating agent and optionally an auxiliary molecule.21. A method of synthesizing radiolabeled benzamides on a solid support comprising:a) selecting a solid support comprising at least one compound attached to said solid support which compound comprises a benzoic acid moiety;b) reacting said moiety of said compound attached to said solid support with at least one amine to afford a benzamide bound to a solid support; andc) reacting said ...

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21-11-2013 дата публикации

METHOD FOR PREPARING 2-AMINOBENZAMIDE DERIVATIVES

Номер: US20130310567A1
Принадлежит: EI DU PONT DE NEMOURS AND COMPANY

A method for preparing a compound of Formula 1 comprising contacting a compound of Formulae 2 and 3 in the presence of a palladium source, a ligand, a base and carbon monoxide 2. The method of wherein Ris C-Calkyl; and Ris Cl or cyano.3. The method of wherein Ris methyl; and Ris chloro.4. The method of wherein Ris methyl; and Ris cyano.5. The method of wherein X is Br.6. The method of wherein Ris H claim 1 , methyl claim 1 , isopropyl or cyclopropylcyclopropyl.7. The of wherein Ris methyl; Ris Cl or cyano; and Ris methyl.8. The method of wherein the base is an organic base comprising a compound of Formula 3; Ris methyl or isopropyl; and the base is in a mole ratio of at least about 2 relative to a compound of Formula 2.9. The method of wherein the palladium source is a palladium(II) species and the ligand is selected from 1 claim 1 ,1′-bis(diphenylphosphino)ferrocene and 1 claim 1 ,4-bis(diphenylphosphino)butane.10. The method of wherein the palladium source is palladium(II) acetate and the ligand is 1 claim 9 ,4-bis(diphenylphosphino)butane.11. The method of wherein the contacting is performed in a suitable solvent comprising ethylene glycol and N claim 1 ,N-dimethylethanolamine.13. The method of wherein the palladium source is a palladium(II) species and the ligand is 1 claim 12 ,1′-bis(diphenylphosphino)ferrocene; and the contacting is performed in a suitable solvent comprising ethylene glycol and N claim 12 ,N-dimethylethanolamine.15. The method of wherein Ris CH; Ris Cl or cyano; Ris CH claim 14 , Ris Br; Ris Cl; Ris H; and Z is N. This invention relates to a method for preparing 2-aminobenzamides and derivatives thereof.Preparation of certain 2-aminobenzamides and their utility as intermediates for preparing insecticidal anthranilic diamides is disclosed in PCT Patent Publication WO 06/062978. However, the need continues for new or improved methods suitable for rapidly and economically providing 2-aminobenzamides and their derivatives.This invention is ...

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28-11-2013 дата публикации

Process for the preparation of lacosamide

Номер: US20130317109A1
Принадлежит: CAMBREX KARLSKOGA AB

There is provided a process for the preparation of Lacosamide (which is a useful medicament) of formula I, which comprises an enantioselective enzymatic acylation.

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28-11-2013 дата публикации

PROCESS FOR PRODUCTION OF AROMATIC AMIDE CARBOXYLIC ACID DERIVATIVE

Номер: US20130317247A1
Принадлежит: MITSUI CHEMICALS AGRO, INC.

The invention provides a method for producing an aromatic amide carboxylic acid derivative represented by the following Formula (2), including a step of reacting an aromatic amide halide derivative represented by the following Formula (1) with carbon monoxide. In the following Formulae (1) and (2), Rrepresents a hydrogen atom or an alkyl group having 1 to 6 carbon atoms; Xrepresents a fluorine atom or a cyano group; Xrepresents a halogen atom; and n represents an integer of from 0 to 3. 5. The aromatic amide halide derivative according to claim 4 , wherein claim 4 , in Formula (1) claim 4 , Rrepresents a methyl group claim 4 , Xrepresents a fluorine atom claim 4 , Xrepresents a chlorine atom claim 4 , and n represents 0 or 1. The invention relates to a method for producing an aromatic amide carboxylic acid derivative.Methods for producing aromatic carboxylic acid derivatives are known in which carbon monoxide is inserted into a certain kind of aromatic halide derivative in the presence of a base and water, using a palladium compound as a catalyst (see, for example, Japanese Patent Application Laid-Open (JP-A) Nos. 8-104661, 2003-48859, and 2005-220107).Furthermore, a method for producing an aromatic amide carboxylic acid derivative having an amide bond and a halogen atom, etc., in the molecule thereof is known (see, for example, International Patent Publication No. WO 2010/18857).The inventors have studied industrial methods for producing aromatic amide carboxylic acid derivatives using the methods described in the above known art. However, the methods require multi-step reactions and are therefore insufficient as industrial production methods.The invention provides a method that allows for the production of an aromatic amide carboxylic acid derivative having a halogen atom, etc., through fewer process steps, and a useful intermediate for use in the production method.As a result of the intensive studies to develop a method that allows for the production of an ...

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12-12-2013 дата публикации

Halogenated Pyrazolo[1,5-A]Pyrimidines, Processes, Uses, Compositions and Intermediates

Номер: US20130331610A1
Принадлежит: Ferrer Internacional, S.A.

The invention provides novel halogenated pyrazolo[1,5-a]pyrimidines of formula (I) wherein R, R, X and Y have different meanings, and pharmaceutically acceptable salts thereof. Compounds of formula (I) are useful for treating or preventing anxiety, epilepsy and sleep disorders including insomnia, and for inducing sedation-hypnosis, anesthesia, sleep and muscle relaxation. The invention also provides synthetic procedures for preparing said compounds and certain intermediates, as well as intermediates themselves. 2. The process of wherein the hydride compound is sodium hydride and Z is iodine.6. An intermediate enaminone compound which is selected from the group consisting of:N-[5-(3-dimethylamino-acryloyl)-2-fluoro-phenyl]-N-methyl-acetamide;N-[2-chloro-5-(3-dimethylamino-acryloyl)-phenyl]-N-methyl-acetamide;N-[5-(3-dimethylamino-acryloyl)-2-fluoro-phenyl]-N-methyl-methanesulfonamide;N-[2-chloro-5-(3-dimethylamino-acryloyl)-phenyl]-N-methyl-methanesulfonamide; andN-[5-(3-dimethylamino-acryloyl)-2-fluoro-phenyl]-N-prop-2-ynyl-methanesulfonamide. This application is a Divisional Application of U.S. patent application Ser. No. 11/922,602, filed Apr. 30, 2009, which is the U.S. National Phase of PCT/EP2006/063243, filed Jun. 15, 2006, which claims benefit of Provisional Application No. 60/692,866 filed on Jun. 21, 2005. This application also claims priority under 35 U.S.C. §119(a) to European Patent Application No. 05105478.1, filed in Europe on Jun. 21, 2005, the entire contents of which are hereby incorporated by reference.This invention is directed to agents with affinity for GABAreceptor, specifically to halogenated pyrazolo[1,5-a]pyrimidines, and more specifically to [7-(3-amino-4-halophenyl)-pyrazolo[1,5-a]pyrimidin-3-yl]-thiophen-2-yl-methanone acyl and sulfonyl compounds.GABAreceptor (γ-aminobutyric acid) is a pentameric protein which forms a membrane ion channel. GABAreceptor is implicated in the regulation of sedation, anxiety, muscle tone, epileptogenic ...

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02-01-2014 дата публикации

NOVEL COMPOUNDS, METHOD FOR PREPARATION THEREOF AND USE THEREOF FOR PREPARING POLYMERS USEFUL FOR INCREASING HEAT RESISTANCE OF POLYMERIC COMPOSITIONS

Номер: US20140005351A1
Принадлежит:

The invention relates to a compound of the following formula (I): to its method for making it and to its uses for preparing a polymer useful for increasing the heat resistance of polymeric compositions. 2. The compound according to claim 1 , wherein p and n are identical and independently represent an integer from 3 to 12 and m represents (n−2).3. The compound according to claim 1 , wherein n claim 1 , m and p are even integers.4. The compound according to claim 1 , wherein m represents 2 or 3.5. The compound according to claim 4 , wherein n and p represent 4 and m represents 2 or n and p represent 5 and m represents 3.7. A method for preparing a (PEA) polymer comprising a step consisting of heating to a temperature greater than or equal to the melting temperature of the compound of formula (I) and under reduced pressure claim 1 , a compound of formula (I) according to claim 1 , in the presence of a catalyst claim 1 , in order to polymerize said compound of formula (I).9. The method for preparing a (PEA) polymer according to claim 1 , wherein the compound of formula (I) is the compound according to .10. A (PEA) polymer obtainable by a method comprising a step consisting of heating a compound of formula (I) according to to a temperature greater than or equal to the melting temperature of said compound of formula (I) and under reduced pressure claim 5 , in the presence of a catalyst claim 5 , in order to polymerize said compound of formula (I).11. A method for improving the heat resistance of a composition claim 10 , comprising the step of adding to said composition a (PEA) polymer according to .12. A composition comprising:{'claim-ref': {'@idref': 'CLM-00010', 'claim 10'}, 'a (PEA) polymer according to ,'}optionally at least one other polymer (P), andoptionally natural fibers.13. A plastic article comprising a composition according to .14. The method for preparing a (PEA) polymer according to claim 8 , wherein the compound of formula (I) is brought into contact with ...

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02-01-2014 дата публикации

Salts and Polymorphs of a Tetracycline Compound

Номер: US20140005420A1
Принадлежит: PARATEK PHARMACEUTICALS, INC.

Crystalline forms, including salts and polymorphs, of a compound useful in the treatment of tetracycline compound-responsive states are provided herein. The crystalline compounds are useful for the treatment or prevention of conditions and disorders such as bacterial infections and neoplasms, as well as other known applications for tetracycline compounds in general. 2. The method of claim 1 , wherein the first solvent or combination of solvents and the second solvent or combination of solvents are the same.3. The method of claim 1 , wherein the first solvent or combination of solvents and the second solvent or combination of solvents are different.4. The method of claim 1 , wherein the first combination of solvents and the second combination of solvents are each independently a combination of alcoholic solvents.5. The method of claim 4 , wherein the first combination of solvents and the second combination of solvents are each independently a combination of two alcoholic solvents.6. The method of claim 5 , wherein the two alcoholic solvents are ethanol and isopropanol.7. The method of claim 6 , wherein the ethanol and isopropanol are at a volume-to-volume ratio of 2 to 1.8. The method of claim 1 , wherein the first combination of solvents and the second combination of solvents each comprises an alcoholic solvent and an anti-solvent.9. The method of claim 8 , wherein the alcoholic solvent is methanol.10. The method of claim 8 , wherein the anti-solvent is selected from a ketone claim 8 , an ester and an ether.11. The method of claim 10 , wherein the ether is methyl-t-butyl ether.12. The method of claim 1 , wherein the first combination of solvents and the second combination of solvents each comprises methanol and methyl-t-butyl ether.13. The method of claim 12 , wherein the methanol and methyl-t-butyl ether are at a volume-to-volume ratio of 1 to 1.2.14. The method of claim 1 , wherein the p-toluenesulfonic acid is provided in an amount of from 25 to 75 wt % relative ...

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09-01-2014 дата публикации

PROCESS FOR PREPARING BICYCLIC AMINE DERIVATIVES

Номер: US20140012015A1
Принадлежит:

The present invention provides a process for preparing a bicyclic amine derivative of the formula (Ia) or (Ib), 2. The process as claims in claim 1 , wherein the rhodium catalyst is a rhodium(I) compound.3. The process as claimed in claim 2 , wherein the rhodium(I) compound is of formula (IIIa) claim 2 , (IIIb) or (IIIc) claim 2 ,{'br': None, 'sup': '1', 'sub': '2', '[RhLiAn]\u2003\u2003(IIIa)'}{'br': None, 'sup': '2', 'sub': 2', 'n, '[RhLiAn]\u2003\u2003(IIIb)'}{'br': None, 'sup': '1', 'sub': '2', '[RhLiAn]\u2003\u2003(IIIc)'}wherein{'sup': '1', 'sub': 5', '12', '5', '12', '5', '12, 'Liis C-C-alkadiene, C-C-cycloalkadiene or C-C-bicycloalkadiene;'}{'sup': '2', 'sub': 2', '12', '5', '8, 'Liis C-C-alkene or C-C-cycloalkene;'}n is 1 or 2; andAn is halide, tetrafluoroborate, trifluoromethanesulfonate or acetylacetonate.4. The process as claimed in claim 3 , wherein the rhodium(I) compound is of formula (IIIa) with Libeing C-C-cycloalkadiene or C-C-bicycloalkadiene claim 3 , in particular 1 claim 3 ,5-cyclooctadiene or norbornadiene claim 3 , and An being chloride.5. The process as claimed in claim 1 , wherein the chiral phosphine ligand is a chiral diphosphine ligand.6. The process as claimed in claim 5 , wherein the diphosphine ligand comprises a ferrocene moiety.8. The process as claimed in claim 7 , wherein the diphosphine ligand is of the formula (IVa) or (IVb) with Rand Rhaving the same meaning and Rand Rhaving the same meaning.9. The process as claimed in claim 8 , wherein Rand Rare both C-C-alkyl and Rand Rare both optionally substituted C-C-hetaryl or optionally substituted C-C-aryl.10. The process as claimed in claim 9 , wherein Rand Rare both tert-butyl and Rand Rare both 1-naphthyl or 2-furyl.12. The process as claimed in claim 9 , wherein the bicyclic amine derivative is a compound of the formula (Ia) and the chiral phosphine ligand is the diphosphine of formula (IVa) claim 9 , as defined in .13. The process as claimed in claim 1 , wherein Xin formulae (Ia) ...

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16-01-2014 дата публикации

CATALYST FOR ASYMMETRIC HYDROGENATION OF IMINE, SYNTHESIS METHOD AND APPLICATION THEREOF

Номер: US20140018548A1
Автор: Li Jin
Принадлежит:

A chiral hydrogenated H-BINOL bisphosphine compound is provided, with the structure shown as the following formula (I), wherein both Rand Rare halogen, H or C-Caliphatic group; Ris H or C-Caliphatic group; Ris halogen, amino, nitro, H, C-Caliphatic group or C-Caromatic group; and X is phenyl, substituted phenyl, cyclohexyl, substituted cyclohexyl, C-Caromatic group, or C-Cheterocyclic aromatic group containing one or more heteroatoms selected from N, S, O. The present invention further provides a catalyst for an asymmetric catalytic hydrogenation reaction which contains the compound, wherein the catalyst can produce more than % of enantiomers and efficiency with the turnover number of greater than in the asymmetric hydrogenation reaction of imines. 4. A catalyst for an asymmetric catalytic hydrogenation reaction claim 1 , characterized by comprising a coordination compound which is an iridium-containing coordination compound formed by the compound as claimed in as a ligand and an iridium-cyclooctadiene complex based on a molar ratio of 0.5-5:1.5. The catalyst as claimed in claim 4 , characterized in that the iridium-cyclooctadiene complex is any one of [IrCl(COD)] claim 4 , [IrBr(COD)]or [Ir(COD)]BF.6. The catalyst as claimed in claim 4 , characterized by further comprising a halogen-containing additive claim 4 , a molar ratio of which to the iridium--containing coordination compound catalyst is 0.001-10:1.7. The catalyst as claimed in claim 6 , characterized in that the halogen-containing additive is selected from an alkali metal salt of a halogen family element claim 6 , a halogen-containing C1-C60 quaternary ammonium salt claim 6 , or a halogen-containing C1-C60 aromatic hydrocarbon or aliphatic hydrocarbon.8. The catalyst as claimed in claim 7 , characterized in that the halogen is chlorine claim 7 , bromine or iodine.9. The catalyst as claimed in claim 7 , characterized in that the halogen-containing additive is selected from iodobenzene claim 7 , tetrabutyl ...

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16-01-2014 дата публикации

Method for Preparing Formamide Compounds

Номер: US20140018576A1

The present invention relates to a method for preparing formamide compounds using carbon dioxide, and to the use of said method for manufacturing vitamins, pharmaceutical products, adhesives, acrylic fibres, synthetic leathers, pesticides and fertilisers. The invention also relates to a method for manufacturing vitamins, pharmaceutical products, adhesives, acrylic fibres, synthetic leathers, pesticides and fertilisers which includes a step of preparing formamide compounds by the method according to the invention. 2. The process as claimed in claim 1 , wherein in the amine of formula (II) claim 1 , Rand Rrepresent independently of one another a hydrogen atom claim 1 , an alkyl group claim 1 , an aryl group claim 1 , a heteroaryl group or an amino group claim 1 , said alkyl claim 1 , amino claim 1 , aryl claim 1 , and heteroaryl groups being optionally substituted claim 1 , or{'sup': 1', '2, 'Rand R, together with the nitrogen atom to which they are bonded, form an optionally substituted heterocycle; or'}{'sup': 1', '2', '6', '6', '7', '6', '7, 'Rand R, with the nitrogen atom to which they are bonded, form a carbon-nitrogen double bond (N═C), thus giving an aldimine of formula —N═CHRor a ketimine of formula —N═CRR, in which Rand Rrepresent independently of one another a hydrogen atom, an alkyl group, an aryl group, a heteroaryl group, or a heterocycle, said alkyl, aryl, heteroaryl, and heterocycle groups being optionally substituted.'}3. The process as claimed in claim 1 , wherein in the silane compound of formula (III) claim 1 , R claim 1 , Rand Rrepresent independently of one another a hydrogen atom claim 1 , an alkyl group claim 1 , an alkoxy group claim 1 , an aryl group claim 1 , a silyl group claim 1 , or a siloxy group claim 1 , said alkyl claim 1 , alkoxy claim 1 , silyl claim 1 , siloxy claim 1 , and aryl groups being optionally substituted.4. The process as claimed in claim 1 , wherein the catalyst is selected from organic catalysts or metal catalysts ...

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23-01-2014 дата публикации

Linezolid intermediate and method for synthesizing linezolid

Номер: US20140024827A1

Provided are a linezolid intermediate and the preparation method thereof and a method for synthesizing linezolid. The structure of the intermediate is shown as formula F2, wherein the compound is prepared by a condensation reaction of (S)—N—(3-chloro-2-hydroxy-1-propyl) acetamide and the compound shown in formula F4. In the preparation methods of the compound shown in formula F2 and linezolid, the reaction system is mild, side reactions are few and the product yield is high.

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30-01-2014 дата публикации

ORGANOZINC COMPLEXES AND PROCESSES FOR MAKING AND USING THE SAME

Номер: US20140031545A1
Принадлежит: LUDWIG-MAXIMILIAN-UNIVERSITAT MUNCHEN

Processes for making an organozinc reagents are disclosed comprising reacting (A) organomagnesium or organozinc complexes with (B) at least one coordination compound comprising one or more carboxylate groups and/or alcoholate groups and/or tertiary amine groups, optionally in combination with zinc ions and/or lithium ions and/or halide ions, wherein the halide ions are selected from chloride, bromide and iodide, the organozinc complex comprises an aryl group, a heteroaryl group or a benzyl group when the coordinating compound is a chelating polyamine, and the reaction is conducted in the presence of zinc complexed with at least one coordinating compound when reactant (A) comprises at least one organomagnesium complex. The resulting organozinc reagents may optionally be isolated from solvents to obtain a solid reagent. The reagents may be used for making organic compounds via Negishi cross-coupling reactions or via aldehyde and/or ketone oxidative addition reactions. The organozinc reagents are stable and, due to their high selectivity, permit maintenance of sensitive functional groups such as aldehydes during cross-coupling. 1. A process for making organozinc reagents comprising:(1) reacting (A) at least one organomagnesium complex or organozinc complex with (B) at least one coordinating compound comprising one or more carboxylate groups and/or alcoholate groups and/or tertiary amine groups, optionally in combination with zinc ions and/or lithium ions and/or halide ions, wherein the halide ions are selected from chloride, bromide and iodide, the organozinc complex comprises an aryl group, a heteroaryl group or a benzyl group when the coordinating compound is a chelating polyamine, and the reaction is conducted in the presence of zinc complexed with at least one coordinating compound when reactant (A) comprises at least one organomagnesium complex,(2) contacting an organic compound having at least one leaving group with magnesium metal and a zinc coordination complex ...

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06-02-2014 дата публикации

Novel process for the preparation of acylguanidines and acylthioureas

Номер: US20140039189A1
Принадлежит: BOEHRINGER INGELHEIM INTERNATIONAL GMBH

The present invention relates to a novel process for the preparation of compounds of general formula (I) and the salts thereof, particularly the physiologically acceptable salts thereof with inorganic or organic acids and bases, which have valuable pharmacological properties, particularly an inhibitory effect on epithelial sodium channels, the use thereof for the treatment of diseases, particularly diseases of the lungs and airways.

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27-02-2014 дата публикации

PREPARATION OF CHIRAL AMIDES AND AMINES

Номер: US20140057990A1
Принадлежит: Sunovion Pharmaceuticals Inc.

This invention provides a convenient method for converting oximes into enamides. The process does not require the use of metallic reagents. Accordingly, it produces the desired compounds without the concomitant production of a large volume of metallic waste. The enamides are useful precursors to amides and amines. The invention provides a process to convert a prochiral enamide into the corresponding chiral amide. In an exemplary process, a chiral amino center is introduced during hydrogenation through the use of a chiral hydrogenation catalyst. In selected embodiments, the invention provides methods of preparing amides and amines that include the 1,2,3,4-tetrahydro-N-alkyl-1-naphthalenamine or 1,2,3,4-tetrahydro-1-naphthalenamine substructure. 1. A method for converting an oxime into an enamide , said method comprising:(a) contacting said oxime with a phosphine and an acyl donor, under conditions appropriate to convert said oxime into said enamide.4. The method according to wherein Ris substituted or unsubstituted aryl.5. The method according to wherein Ris substituted or unsubstituted phenyl.6. The method according to wherein Ris phenyl substituted with at least one halogen.8. The method according to wherein Xand Xare each chloro.9. The method according to wherein Ar is substituted or unsubstituted phenyl.11. The method according to wherein said acyl donor has the formula:{'br': None, 'sup': '5', 'Z—C(O)—R'} Z is a leaving group; and', {'sup': '5', 'Ris a member selected from H, substituted or unsubstituted alkyl, substituted or unsubstituted heteroalkyl, substituted or unsubstituted aryl, substituted or unsubstituted heteroaryl and substituted or unsubstituted heterocycloalkyl.'}], 'wherein'}12. The method according to wherein Z has the formula:{'br': None, 'sup': '6', 'R—C(O)—O—'} {'sup': '6', 'Ris a member selected from substituted or unsubstituted alkyl, substituted or unsubstituted heteroalkyl, substituted or unsubstituted aryl, substituted or unsubstituted ...

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27-02-2014 дата публикации

SYSTEM FOR FLUORINATING ORGANIC COMPOUNDS

Номер: US20140058106A1
Принадлежит:

Described herein are fluorinated organic compounds and methods of making fluorinated organic compounds, for example, using palladium complexes. Also described herein are compositions and kits containing compounds and palladium complexes described herein. 2. The palladium complex of claim 1 , wherein the palladium complex further comprises a negatively charged counterion X claim 1 , wherein X is selected from BF claim 1 , BPh claim 1 , PF claim 1 , [BArF] claim 1 , B(CF) claim 1 , SbF claim 1 , and CFSO.3. The palladium complex of claim 1 , wherein Z is —N(R)—.4. The palladium complex of claim 3 , wherein Ris —S(O)R.5. The palladium complex of claim 4 , wherein Ris optionally substituted aryl.7. The palladium complex of claim 1 , wherein Ris pyridyl.8. The palladium complex of claim 1 , wherein Ris halogen claim 1 , an optionally substituted heteroaryl claim 1 , or —OR.9. The palladium complex of claim 8 , wherein Ris —Cl or pyridyl.10. The palladium complex of claim 1 , wherein Ris —C(═O)Ror —S(O)R.11. The palladium complex of claim 10 , wherein Ris an optionally substituted aliphatic.12. The palladium complex of claim 11 , wherein Ris —C(═O)CHor —S(O)CF.15. The method of claim 14 , wherein the organic compound comprises an aryl group.16. The method of claim 14 , wherein the organic compound comprises a boron substituent.18. The method of claim 14 , wherein the fluorinating agent provides a source of F.20. The palladium complex of claim 19 , wherein Ris pyridyl.21. The palladium complex of claim 19 , wherein Ris halogen claim 19 , an optionally substituted heteroaryl claim 19 , or —OR.22. The palladium complex of claim 21 , wherein Ris —Cl or pyridyl.23. The palladium complex of claim 21 , wherein Ris —C(═O)Ror —S(O)R.24. The palladium complex of claim 23 , wherein Ris an optionally substituted aliphatic.25. The palladium complex of claim 24 , wherein Ris —C(═O)CHor —S(O)CF. The present application is a Continuation of U.S. application Ser. No. 12/865,703, which is ...

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20-03-2014 дата публикации

METHOD OF PREPARINGIODOOCTYL FENBUFEN AMIDE AND APPLICATION THEREOF

Номер: US20140079633A1
Принадлежит: National Tsing Hua University

The present invention provides a method of preparing [I]Iodooctyl fenbufen amide with a radiochemical yield of 15%, a specific activity of 37 GBq/μmol and radiochemical purity of 95%. The present invention further provides a method of applying [I]Iodooctyl fenbufen amide as tracer of single photon emission computer tomography (SPECT) to estimate the distribution of cyclooxygenase. By the binding characteristics of the iodine isotope-labeled compounds and the positive correlation of inflammation to tumor lesion, the present invention can estimate the tumor development and metastasis. 2. The method according to claim 1 , wherein the stannyl compound is hexamethylditin (Sn(CH)).3. The method according to claim 1 , wherein the I-labeled Iodine reagent is I-labeled sodium iodide.5. The method according to claim 1 , wherein the compound of formula 1 is used as a tracer of an image-forming system.6. A method of detecting the early inflammatory lesion of a tumor by using the compound of formula 1 according to as a tracer of an image-forming system claim 1 , comprising combining the compound of formula 1 with cyclooxygenase to produce a signal claim 1 , wherein the cyclooxygenase is cyclooxygenase-1 (COX-1) or cyclooxygenase-2 (COX-2).7. The method according to claim 6 , wherein the image-forming system is a single photon emission tomography (SPECT).8. The method according to claim 6 , wherein the tumor is a liver tumor.9. The method according to claim 6 , wherein the signal is a hot spot displayed by radioactive accumulation.10. The method according to claim 9 , wherein the hot spot is positively correlated to the tumor lesion. This application claims the priority benefit of Taiwan application serial no. 101134033, filed on 17 Sep. 2012. The disclosure of the Taiwan application is incorporated by reference herein.1. Field of the InventionThe present invention relates to a method of preparing [I]Iodooctyl fenbufen amide and application.2. The Prior ArtsNon steroid anti ...

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04-01-2018 дата публикации

POLYMORPHIC AND AMORPHOUS FORMS OF (R)-2-HYDROXY-2-METHYL-4-(2,4,5-TRIMETHYL-3,6-DIOXOCYCLOHEXA-1,4-DIENYL)BUTANAMIDE

Номер: US20180000749A1
Принадлежит:

Disclosed herein are polymorphic and amorphous forms of anhydrate, hydrate, and solvates of (R)-2-hydroxy-2-methyl-4-(2,4,5-trimethyl-3,6-dioxocyclohexa-1,4-dienyl)butanamide and methods of using such compositions for treating or suppressing oxidative stress disorders, including mitochondrial disorders, impaired energy processing disorders, neurodegenerative diseases and diseases of aging. Further disclosed are methods of making such polymorphic and amorphous forms. 1. An polymorph of an anhydrate , a hydrate , or a solvate of (R)-2-hydroxy-2-methyl-4-(2 ,4 ,5-trimethyl-3 ,6-dioxocyclohexa-1 ,4-dienyl)butanamide , wherein the polymorph is selected from the group consisting of Forms I-VI as described in Table A or Tables 2-7 respectively.2. The polymorph of claim 1 , wherein the polymorph is Form I claim 1 , wherein a powder X-ray diffraction pattern for the polymorph comprises characteristic peaks at the following angular positions claim 1 , wherein the angular positions may vary by ±0.2: 12.06 claim 1 , 17.03 claim 1 , and 17.26.3. The polymorph of claim 1 , wherein the polymorph is Form I claim 1 , wherein a powder X-ray diffraction pattern for the polymorph comprises characteristic peaks at the following angular positions claim 1 , wherein the angular positions may vary by ±0.2: 12.06 claim 1 , 15.33 claim 1 , 17.03 claim 1 , 17.26 claim 1 , and 18.72.4. The polymorph of claim 1 , wherein the polymorph is Form I claim 1 , wherein the polymorph has a powder x-ray diffraction pattern substantially as shown in .5. A composition comprising the polymorph of any one of - claim 1 , wherein the composition is essentially free of Forms II-VI claim 1 , wherein Forms II-VI are described in Table A or Tables 3-7 respectively.6. A composition comprising the polymorph of any one of - claim 1 , wherein at least about 95% by mole of the composition is the polymorph Form I claim 1 , exclusive of any solvents claim 1 , carriers or excipients.7. The polymorph of claim 1 , wherein ...

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03-01-2019 дата публикации

Biobased Carbon Fibers and Carbon Black and Methods of Making the Same

Номер: US20190002293A1
Принадлежит: NOVOMER, INC.

Bio-based materials, e.g., epoxide starting material, a beta-lactone starting material and/or a beta-hydroxy amide starting material, may be used as feedstocks in processes for making and using acrylonitrile and acrylonitrile derivatives to produce, among other products, carbon fibers and carbon black. 1. A method of producing a carbon fiber material , the method comprising:a. affording acrylonitrile from at least one of an epoxide or carbon monoxide starting material that is derived from a bio-based and/or renewable source;b. polymerizing the acrylonitrile to produce a polyacrylonitrile precursor;c. thermally stabilizing the polyacrylonitrile precursor to afford thermally stabilized carbon fibers; andd. carbonizing the thermally stabilized carbon fibers to produce the carbon fiber material.2. The method from claim 1 , wherein the acrylonitrile is produced by a process comprising:a. introducing the at least one of bio-based and/or renewable sourced epoxide and carbon monoxide starting materials to at least one reaction vessel through at least one feed stream inlet;b. contacting the at least one of bio-based and/or renewable sourced epoxide and carbon monoxide starting materials with a carbonylation catalyst in the at least one reaction vessel to produce a beta-lactone intermediate;c. contacting the beta-lactone intermediate with a heterogenous catalyst to produce an organic acid intermediate; andd. reacting the organic acid product with an ammonia reagent under ammoxidation conditions in the at least one reaction vessel to produce the acrylonitrile product.3. The method from claim 1 , wherein the polyacrylonitrile precursor comprises polyacrylonitrile fibers produced by wet or dry-jet-wet spinning of an acrylonitrile monomer or copolymer.4. The method from claim 1 , wherein polyacrylonitrile precursor is thermally stabilized by controlled low-temperature heating over the range 200-300° C. in air.5. The method from claim 1 , wherein the carbon fiber material is ...

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02-01-2020 дата публикации

METHOD FOR THE ONE-POT PRODUCTION OF ORGANO-IODINATED COMPOUNDS

Номер: US20200002269A1
Принадлежит:

The present invention concerns a process for the preparation of organo-iodized compounds, as well as their preparation intermediates. More particularly, the present invention concerns a process for the preparation of organo-iodized compounds which can be used as preparation intermediates in the synthesis of iodized contrast agents. 19-. (canceled)11. The process of claim 10 , wherein the steps a) and b) are carried out in a single reactor.13. The process of claim 10 , wherein steps a) and b) are carried out in the presence of a solvent selected from the group consisting of dimethylacetamide claim 10 , propylene carbonate claim 10 , acetonitrile claim 10 , tetrahydrofuran claim 10 , and mixtures thereof.14. The process of claim 10 , wherein step b) is carried out in the presence of a chlorination agent selected from the group consisting of thionyl chloride claim 10 , phosphorus oxychloride claim 10 , phosphorus trichloride claim 10 , oxalyl chloride claim 10 , phosphorus pentachloride claim 10 , and methanoyl dichloride. The present invention relates to a process for the preparation of organo-iodized compounds, as well as their preparation intermediates. More precisely, the present invention relates to a process for the preparation of organo-iodized compounds used as preparation intermediates in the synthesis of iodized contrast agents.Currently, the majority of processes for the synthesis of iodized contrast agents use the dichloride of 5-amino-2,4,6-triiodoisophthalic acid (also known as DiCOCl), with the following formula:This compound is used in particular as an intermediate product in the synthesis of many contrast agents such as iopamidol (Iopamiron®), iohexol (Omnipaque®), ioversol (Optiray®), iomeprol (Iomeron®) or iobitridol (Xenetix®).During the synthesis of iodized contrast agents, it is necessary to carry out lengthy steps for separation and purification in order to obtain synthesis intermediates with a good level of purity. These steps considerably ...

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03-01-2019 дата публикации

Methods and systems for mask alignment in manufacturing process of arrays

Номер: US20190002410A1
Принадлежит: HealthTell Inc

Provided herein are molecules and salts thereof, arrays containing molecules and salts thereof, solid supports containing molecules and salts thereof, kits containing molecules or salts thereof, and methods of determining alignment of photolithographic masks comprising molecules or salts thereof.

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02-01-2020 дата публикации

Process for making hepatitis b core protein modulators

Номер: US20200002325A1
Принадлежит: Assembly Biosciences Inc

The present disclosure provides, in part, a process for preparing compounds (I) having allosteric effector properties against Hepatitis B virus Cp.

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20-01-2022 дата публикации

L-DOPA AND/OR DOPA DECARBOXYLSE INHIBITORS CONJUGATED TO SUGAR FOR THE TREATMENT OF DOPAMINE-RESPONSIVE DISORDERS

Номер: US20220016253A1

The present invention provides conjugates comprising a sugar such as mannitol and one or more L-DOPA and/or DOPA decarboxylse inhibitors including, inter alia, L-DOPA, carbidopa, benserazide, or a combination thereof, wherein the sugar is conjugated to the carboxyl group of the L-DOPA and/or DOPA decarboxylse inhibitor/ s) via a hydroxyl group of the sugar. The present invention further provides related pharmaceutical compositions and methods of producing the conjugates, as well as methods of use for treating medical disorders responsive to dopamininergic stimulation such as movement disorders including, inter alia, Parkinson's Disease. 170.-. (canceled)71. A conjugate comprising a sugar and one or more a) L-DOPA molecules; b) inhibitors of DOPA decarboxylase; or c) a combination of L-DOPA molecules and inhibitors of DOPA decarboxylase , wherein said sugar is conjugated a) to the carboxyl group of each of said L-DOPA molecules; b) to the carboxyl group of the DOPA decarboxylase inhibitor; or c) to the carboxyl group of a spacer bound to said one or more inhibitors of DOPA decarboxylase , via a hydroxyl group of said sugar.72. The conjugate of claim 71 , wherein said conjugate comprises one molecule of mannitol and 1-4 molecules of L-DOPA; one molecule of mannitol and 1-6 molecules of the DOPA decarboxylase inhibitor claim 71 , one molecule of mannitol claim 71 , four molecules of L-DOPA claim 71 , and one molecule of carbidopa; or a combination thereof.73. The conjugate of claim 71 , wherein said inhibitor of DOPA decarboxylase comprises carbidopa claim 71 , methyldopa claim 71 , alpha-Difluoromethyl-DOPA (DFMD) claim 71 , or a combination thereof.74. The conjugate of claim 71 , wherein said inhibitor of DOPA decarboxylase comprises benserazide and wherein said spacer comprises a dicarboxylic acid.75. The conjugate of claim 71 , wherein said sugar comprises mannitol claim 71 , glucose claim 71 , or galactose.76. A pharmaceutical composition comprising one or more ...

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14-01-2016 дата публикации

3'-substituted-abscisic acid derivatives

Номер: US20160007598A1
Принадлежит: Valent BioSciences LLC

The invention relates to a novel class of (S)-3′-substituted-abscisic acid derivatives and (±)-3′-substituted-abscisic acid derivatives, and methods of synthesizing the derivatives.

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12-01-2017 дата публикации

BRANCHED CHAIN-CONTAINING AROMATIC COMPOUND

Номер: US20170008922A1
Автор: TAKAHASHI Daisuke
Принадлежит: AJINOMOTO CO., INC.

The present invention provides a particular branched chain-containing aromatic compound. The branched chain-containing aromatic compound of the present invention is easily-soluble in isopropyl acetate superior in liquid-separation operability, and can be used for a production method of peptide and the like, which provides a final product simply by extraction separation, without crystallization and isolation of each intermediate in each step. 125-. (canceled)2831-. (canceled) The present invention relates to an aromatic compound containing a particular branched chain. The present invention further relates to a protecting reagent containing the compound or an adduct thereof. The present invention also relates to a production method of peptide by using the compound, and further relates to an organic synthesis method including the production method of the peptide.The production methods of peptide are generally divided into solid phase methods and liquid phase methods. The solid phase methods are advantageous since isolation and purification after reaction can be performed by only washing resin. However, they are associated with problems in that the reaction is essentially that of heterogeneous phases, reaction agents and reagents need to be used in excess to compensate for the low reactivity, and tracing of reaction and analysis of reaction product supported by carrier are difficult. On the other hand, the liquid phase method is advantage since it shows good reactivity, and intermediate peptide can be purified by extraction and washing, isolation and the like after condensation reaction. However, the method is associated with problems since the production step is complicated due to an extraction and washing step with a nonpolar organic solvent and an acidic or basic aqueous solution to remove residual reagents and/or byproducts in each step of coupling reaction and deprotection, and/or an isolation and purification step such as crystallization and the like, and the like ...

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14-01-2016 дата публикации

AMINE-CONTAINING LIPIDS AND USES THEREOF

Номер: US20160009657A1
Принадлежит: Massachusetts Institute of Technology

Nitrogen-containing lipids prepared from the conjugate addition of amines to acrylates, acrylamides, or other carbon-carbon double bonds conjugated to electron-withdrawing groups are described. Methods of preparing these lipids from commercially available starting materials are also provided. These amine-containing lipids or salts forms of these lipids are preferably biodegradable and biocompatible and may be used in a variety of drug delivery systems. Given the amino moiety of these lipids, they are particularly suited for the delivery of polynucleotides. Complexes or nanoparticles containing the inventive lipid and polynucleotide have been prepared. The inventive lipids may also be used to in preparing microparticle for drug delivery. They are particularly useful in delivering labile agents given their ability to buffer the pH of their surroundings. 36-. (canceled)7. The compound of claim 1 , wherein each occurrence of Rand Ris hydrogen.10. (canceled)1213-. (canceled)1516-. (canceled)1819-. (canceled)2125-. (canceled)30. (canceled)31. The compound of claim 29 , wherein Rand Rare C-Cstraight chain alkyl groups.3250-. (canceled)5382-. (canceled)8495-. (canceled)96. A microparticle claim 1 , liposome claim 1 , or micelle comprising a compound of and an agent to be delivered.97108-. (canceled)109. A pharmaceutical composition comprising a compound of and pharmaceutical agent.110111-. (canceled)113131-. (canceled) The present application is a continuation of and claims priority under 35 U.S.C. §120 to U.S. application Ser. No. 11/453,222, filed Jun. 14, 2006, now U.S. Pat. No. 9,006,487, which claims priority under 35 U.S.C. §119(e) to U.S. provisional patent applications, U.S. Ser. No. 60/690,608, filed Jun. 15, 2005, and U.S. Ser. No. 60/785,176, filed Mar. 23, 2006, each of which is incorporated herein by reference.This invention was made with Government support under Grant No. R01-EB000244 awarded by the National Institutes of Health. The Government has certain ...

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27-01-2022 дата публикации

SYNTHESIS OF A CATIONIC SURFMER AND ITS COPOLYMERS FOR ENHANCED OIL RECOVERY

Номер: US20220025090A1
Автор: Han Ming, Xu Limin, Zhang Xuan
Принадлежит: Saudi Arabian Oil Company

Provided is a quaternary ammonium surfmer, that may have the following general formula (I): N—RRRR(X), where: Rand Rmay independently be H or a C-Calkyl, Rmay be a C amidoalkyl group, Rmay be a C-Calkyl having a terminal olefin double bond group, and X may be a halogen. Further provided is a method for synthesizing the quaternary ammonium surfmer and a method for recovering hydrocarbons from a subterranean formation that may include injecting a treatment fluid comprising the quaternary ammonium surfmer into the subterranean formation. 1. A quaternary ammonium surfmer , having the following general formula (I){'br': None, 'sup': +', '1', '2', '3', '4', '−, 'N—RRRR(X)\u2003\u2003(I)'}where:{'sup': 1', '2, 'sub': 1', '3, 'Rand Rare independently H or a C-Calkyl,'}{'sup': '3', 'sub': '19+', 'Ris a C amidoalkyl group,'}{'sup': '4', 'sub': 3', '6, 'Ris a C-Calkyl having a terminal olefin double bond group, and'}X is a halogen.2. The quaternary ammonium surfmer of claim 1 , wherein Ris an erucyl-amidoalkyl group.3. The quaternary ammonium surfmer of claim 2 , wherein Ris an erucyl-amidopropyl group.4. The quaternary ammonium surfmer of claim 1 , wherein Rand Rare each a methyl group.5. The quaternary ammonium surfmer of claim 1 , wherein Ris an allyl group (—CH—CH═CH).6. The quaternary ammonium surfmer of claim 1 , wherein X is bromide or chloride.7. The quaternary ammonium surfmer of claim 1 , having the following general formula (II):{'br': None, 'sup': 5', '6', '7', '+', '1', '2', '4', '−, 'R—CH═CH—R—COHN—R—NRRR(Br)\u2003\u2003(II)'}where:{'sup': '5', 'sub': 8', '16, 'Ris a C-Calkyl,'}{'sup': '6', 'sub': 9', '16, 'Ris a C-Calkyl,'}{'sup': '7', 'sub': 2', '6, 'Ris a C-Calkyl, and'}{'sup': 1', '2', '4, 'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, 'R, R, and Rare as defined in .'}8. The quaternary ammonium surfmer of claim 7 , wherein Ris a Calkyl claim 7 , Ris a Calkyl claim 7 , Ris propyl claim 7 , Rand Rare each methyl claim 7 , and Ris an allyl group (—CH—CH═CH) or ...

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11-01-2018 дата публикации

Ligand-Enabled meta-C-H Activation Using a Transient Mediator

Номер: US20180009739A1
Автор: YU JIN-QUAN
Принадлежит:

An alternative approach to formation of a C-C bond at a meta-position of an aromatic compound is disclosed that employs an ethylenically unsaturated bicyclic compound as a transient mediator to achieve meta-selective C-H activation with a simple and common ortho-directing group. The use of a pyridine-based ligand assists in relaying the palladium catalyst to the meta-position by the unsaturated bicyclic compound following initial ortho-C-H activation. 2. The method according to claim 1 , wherein circled Ar is carbocyclic.3. The method according to claim 2 , wherein one or both of Vand Vare other than hydrido.4. The method according to claim 3 , wherein Z is C.5. The method according to claim 4 , wherein W is C and X is ═O.6. The method according to claim 4 , wherein Ris a 4-(CF)CFNH— group.7. The method according to claim 4 , wherein Ris H.8. The method according to claim 4 , wherein Ris HY.9. The method according to claim 4 , wherein Ris HR.10. The method according to claim 1 , wherein W is nitrogen that is a ring atom of an aromatic ring system that contains at least one additional nitrogen atom that is adjacent to W in the aromatic ring.11. The method according to claim 1 , wherein W is the carbon of a >CH— group claim 1 , X is a N-sulfonamido or N-carboxamido group claim 1 , and Ris a C-C-hydrocarbyl carboxylate group.12. The method according to claim 1 , wherein W is C and W claim 1 , X and Rtogether form a heteroaromatic ring structure that contains one ring or two fused rings that each contains 5- or 6-members and a total of one to four heteroatoms that are independently nitrogen claim 1 , oxygen or sulfur.13. The method according to claim 1 , wherein said reactive coupling agent is an aromatic claim 1 , benzylic or aliphatic bromide or iodide compound of the Formula R-Q claim 1 , wherein Ris an aromatic group claim 1 , a straight claim 1 , branched or cyclic aliphatic C-C-hydrocarbyl group claim 1 , or a benzylic group claim 1 , and Q is bromo or iodo.14. ...

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08-01-2015 дата публикации

PROCESS FOR THE PREPARATION OF ALISKIREN

Номер: US20150011793A1
Принадлежит: MYLAN LABORATORIES LTD

The present invention relates to an improved process for the preparation of pure compound of Formula-II, which is an intermediate in the preparation of Aliskiren and further conversion of compound of Formula-II into Aliskiren or its pharmaceutically acceptable salts. 2. The process according to claim 1 , wherein methylating agent is selected from methyl iodide or dimethyl sulfate.3. The process of according to claim 1 , where in methylation is carried out optionally in presence of phase transfer catalyst.4. The process according to claim 3 , wherein phase transfer catalyst is selected from tertramethyl ammonium bromide claim 3 , tetrabutyl ammonium bromide claim 3 , methyl triethyl ammonium bromide claim 3 , benzyl trimethyl ammonium bromide claim 3 , benzyl triethyl ammonium bromide claim 3 , molecular sieves or crown ethers.5. The process according to claim 1 , wherein methylation is carried out in presence of base.6. The process according to claim 5 , wherein the base is selected from alkali metal hydroxides or alkali metal alkoxides.7. The process according to claim 6 , wherein the base is sodium hydroxide claim 6 , potassium hydroxide or sodium methoxide.8. The process according to claim 1 , wherein compound of Formula-II is further converted into Aliskiren or it's pharmaceutically acceptable salts.10. The process according to claim 9 , wherein methylating agent is selected from methyl iodide or dimethyl sulfate. The present invention relates to an improved process for the preparation of renin inhibitor Aliskiren intermediates and further conversion into Aliskiren and its pharmaceutically acceptable salts.Aliskiren, (2S, 4S, 5S, 7S)-N-(2-carbamoyl-2-methylpropyl)-5-amino-4-hydroxy-2,7-diisopropyl-8-[4-methoxy-3-(3-methoxypropoxy)phenyl] octanamide having the Formula-I, a new antihypertensive has been developed which interferes with the renin-angiotensin system at the beginning of angiotensin II biosynthesis.Aliskiren is marketed by Novartis as TEKTURNA® in the ...

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08-01-2015 дата публикации

Ketoxime- and amide-functionalized nanomaterials

Номер: US20150011794A1
Принадлежит: US Air Force

Ketoxime- and amide-functionalized nanomaterials. The nanomaterials including a nanomaterial comprising a carbon nanotube or a carbon nanofiber. At least one ketoxime group coupled to a first location on the nanomaterial, and at least one amide group coupled to a second location on the nanomaterial.

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09-01-2020 дата публикации

PROCESS FOR THE PREPARATION OF BIMATOPROST

Номер: US20200010406A1
Принадлежит:

It is provided a process for the preparation of bimatoprost, which comprises: a) reacting a compound of formula (III) with ethylamine in the presence of a suitable solvent; and b) deprotecting compound obtained in step a) to obtain bimatoprost, wherein Ris selected from (C-C)alkyl, (CC)haloalkyl, (C-C)alkenyl, (C-C)haloalkenyl, (C-C)alkoxy(C-C)alkyl, aryl, (C-C)alkylaryl, allyl, —(CH—CH—O)—CHwherein n=1, 2, 3 or 4, and —CH(O—CH—CH); Ris selected from H, (C-C)alkyl, (C-C)haloalkyl, (C-C)alkenyl, (C-C)haloalkenyl, (C-C)alkoxy(CrC)alkyl, aryl, (C-C)alkylaryl, allyl; or, alternatively, Rand Rtaken together are selected from —CH—CH—CH—, —CH—CH—, —O—CH—CH—, and —O—CH═CH—. There are also provided intermediates useful in such preparation process. 2. The process according to claim 1 , wherein Ris a (C-C)alkyl and Ris H.3. The process according to claim 2 , wherein Ris selected from ethyl and n-butyl and Ris H.4. The process according to claim 1 , wherein Rand Rtaken together are selected from the group consisting of —CH—CH—CH— claim 1 , —CH—CH— claim 1 , —O—CH—CH— claim 1 , and —O—CH═CH—.5. The process according to claim 4 , wherein Rand Rtaken together are —CH—CH—CH—.6. The process according to claim 1 , wherein step a) is carried out at a temperature from 0 to 100° C.9. The compound according to claim 8 , wherein Ris a (C-C)alkyl and Ris H; or claim 8 , alternatively claim 8 , Rand Rtaken together are selected from the group consisting of —CH—CH—CH— claim 8 , —CH—CH— claim 8 , —O—CH—CH— claim 8 , and —O—CH═CH—.10. The compound according to claim 9 , wherein Ris selected from ethyl and n-butyl and Ris H; or claim 9 , alternatively claim 9 , Rand Rtogether are —CH—CH—CH—.13. The compound according to claim 12 , wherein Ris a (C-C)alkyl and Ris H; or claim 12 , alternatively claim 12 , Rand Rtogether are selected from the group consisting of —CH—CH— claim 12 , —O—CH—CH— claim 12 , and —O—CH═CH—.14. The compound according to claim 13 , wherein Ris selected from ethyl and n- ...

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11-01-2018 дата публикации

Resin, photosensitive resin composition, electronic component and display device using the same

Номер: US20180011402A1
Принадлежит: TORAY INDUSTRIES INC

A resin having a small linear thermal expansion coefficient and a low absorbance is provided. The resin is characterized by including at least one structure selected from structures represented by the following general formulae (1) and (2):

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03-02-2022 дата публикации

Anionic-cationic-nonionic surfactant, production and use thereof

Номер: US20220033705A1

An anionic-cationic-nonionic surfactant as substantially represented by the formula (I) exhibits significantly improved interfacial activity and stability as compared with the prior art. With the present anionic-cationic-nonionic surfactant, a flooding fluid composition for tertiary oil recovery with improved oil displacement efficiency and oil washing capability as compared with the prior art could be produced. In the formula (I), each group is as defined in the specification.

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21-01-2016 дата публикации

An Improved Process for the Synthesis of Melphalan and the Hydrochloride Salt

Номер: US20160016889A1
Принадлежит:

The present invention relates to an improved process for the preparation of Melphalan, more specifically the invention relates to an efficient process for the preparation of substantially pure Melphalan hydrochloride (I).

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21-01-2016 дата публикации

PREPARATION OF CHIRAL AMIDES AND AMINES

Номер: US20160016891A1
Принадлежит:

This invention provides a convenient method for converting oximes into enamides. The process does not require the use of metallic reagents. Accordingly, it produces the desired compounds without the concomitant production of a large volume of metallic waste. The enamides are useful precursors to amides and amines. The invention provides a process to convert a prochiral enamide into the corresponding chiral amide. In an exemplary process, a chiral amino center is introduced during hydrogenation through the use of a chiral hydrogenation catalyst. In selected embodiments, the invention provides methods of preparing amides and amines that include the 1,2,3,4-tetrahydro-N-alkyl-1-naphthalenamine or 1,2,3,4-tetrahydro-1-naphthalenamine substructure.

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21-01-2016 дата публикации

GOLD COMPLEXES

Номер: US20160016976A2
Автор: NOLAN Steven P.

Gold (I) hydroxide complexes of the form Z—Au—OH and digold complexes of the form Z—Au-(μOH)—Au—Z where groups Z are two electron donors are provided. The groups Z may be carbenes, for example nitrogen containing heterocyclic carbenes (NHCs), phosphines or phosphites. The complexes can be used as catalysts, for example in reactions such as hydration of nitriles, skeletal arrangement of enynes, alkoxycyclisation of enynes, alkyne hydration, the Meyer-Shuster reaction, 3,3′ rearrangement of allylic acetates, cyclisation of propargylic acetates, Beckman rearrangements and hydroamination. The complexes can be used in medicine, for example in the treatment of cancer. 2. The method according to wherein the complex is used as a catalyst claim 1 , or for the in situ production of a catalyst claim 1 , for catalyzing a chemical transformation of the substrate claim 1 , the chemical transformation selected from the group consisting of: hydration of nitriles claim 1 , skeletal arrangement of enynes claim 1 , alkoxycyclisation of enynes claim 1 , alkyne hydration claim 1 , the Meyer-Shuster reaction claim 1 , 3 claim 1 ,3′ rearrangement of allylic acetates claim 1 , cyclisation of propargylic acetates claim 1 , Beckman rearrangements and hydroamination.3. (canceled)4. (canceled)5. The method according to wherein the complex is according to general formula V and the anion A is selected from the group consisting of BF claim 1 , PF claim 1 , SbF claim 1 , [B{CH(CF)}] claim 1 , and [B(CF)].6. The method according to wherein the groups Z are selected from the group consisting of carbene claim 1 , phosphine claim 1 , and phosphite two-electron donor ligands.7. The method according to wherein the groups Z are selected from the group consisting of cyclic or acyclic carbenes having one or more heteroatoms claim 6 , triphenylphosphine claim 6 , substituted triphenylphenylphosphine claim 6 , substituted triphenylphosphite claim 6 , and substituted triphenyl phosphite.8. The method ...

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18-01-2018 дата публикации

PREPARATION OF CHIRAL AMIDES AND AMINES

Номер: US20180016224A1
Принадлежит:

This invention provides a convenient method for converting oximes into enamides. The process does not require the use of metallic reagents. Accordingly, it produces the desired compounds without the concomitant production of a large volume of metallic waste. The enamides are useful precursors to amides and amines. The invention provides a process to convert a prochiral enamide into the corresponding chiral amide. In an exemplary process, a chiral amino center is introduced during hydrogenation through the use of a chiral hydrogenation catalyst. In selected embodiments, the invention provides methods of preparing amides and amines that include the 1,2,3,4-tetrahydro-N-alkyl-1-naphthalenamine or 1,2,3,4-tetrahydro-1-naphthalenamine sub structure. 151.-. (canceled) This application claims priority under 35 U.S.C. §119(e) to U.S. Provisional Patent Application No. 60/787,837 filed Mar. 31, 2006, which application is incorporated herein by reference in its entirety for all purposes.This invention relates to processes suitable for the large-scale preparation of enantiomerically- or diastereomerically-enriched chiral amides and amines prepared by these processes.Enantiomerically-enriched chiral primary amines are commonly used as resolving agents for racemic acids, as chiral auxiliaries for asymmetric syntheses and as ligands for transition metal catalysts used in asymmetric catalysis. In addition, many pharmaceuticals, such as sertraline, contain chiral amine moieties. Effective methods for the preparation of such compounds are of great interest to the pharmaceutical industry. Particularly valuable are processes that allow for the preparation of each enantiomer or diastereomer, in enantiomeric or diastereomeric excess, as appropriate, from prochiral or chiral starting materials.Methods are available for the preparation of enantiomerically enriched amines. For example, the addition of organometallic reagents to imines or their derivatives is reported by Watanabe et al., . ...

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21-01-2021 дата публикации

POLYMORPHIC AND AMORPHOUS FORMS OF (R)-2-HYDROXY-2-METHYL-4-(2,4,5-TRIMETHYL-3,6-DIOXOCYCLOHEXA-1,4-DIENYL)BUTANAMIDE

Номер: US20210015765A1
Принадлежит:

Disclosed herein are polymorphic and amorphous forms of anhydrate, hydrate, and solvates of (R)-2-hydroxy-2-methyl-4-(2,4,5-trimethyl-3,6-dioxocyclohexa-1,4-dienyl)butanamide and methods of using such compositions for treating or suppressing oxidative stress disorders, including mitochondrial disorders, impaired energy processing disorders, neurodegenerative diseases and diseases of aging. Further disclosed are methods of making such polymorphic and amorphous forms. 1. A polymorph of a solvate of (R)-2-hydroxy-2-methyl-4-(2 ,4 ,5-trimethyl-3 ,6-dioxocyclohexa-1 ,4-dienyl)butanamide , wherein the polymorph is selected from the group consisting of Forms IV , V , and VI wherein a powder X-ray diffraction pattern for polymorph Form IV comprises characteristic peaks at least at the following angular positions , wherein the angular positions may vary by ±0.2: 4.31 , 12.97 , and 13.20; wherein a powder X-ray diffraction pattern for polymorph Form V comprises characteristic peaks at least at the following angular positions , wherein the angular positions may vary by ±0.2: 9.61 , 11.49 , and 15.45; and wherein a powder X-ray diffraction pattern for polymorph Form VI comprises characteristic peaks at least at the following angular positions , wherein the angular positions may vary by ±0.2: 6.27 , 9.91 , and 12.94.26.-. (canceled)7. The polymorph of claim 1 , wherein the polymorph is Form V.8. The polymorph of claim 1 , wherein the polymorph is Form V claim 1 , wherein a powder X-ray diffraction pattern for the polymorph comprises characteristic peaks at the following angular positions claim 1 , wherein the angular positions may vary by ±0.2: 9.61 claim 1 , 11.49 claim 1 , 12.93 claim 1 , 15.45 claim 1 , and 26.05.9. (canceled)10. A composition comprising the polymorph claim 7 , wherein the composition is essentially free of Forms I-IV and VI claim 7 , wherein; wherein a powder X-ray diffraction pattern for polymorph Form I comprises characteristic peaks at least at the ...

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17-01-2019 дата публикации

PROCESS FOR THE CO-PRODUCTION OF LONG CHAIN AMINO ACIDS AND DIBASIC ACIDS

Номер: US20190016668A1
Автор: HU Songzhou
Принадлежит: Xirui Technology (Beijing) Co., Ltd

There is disclosed a process for the co-production of long chain ω-amino acid and long chain dibasic acid, comprising: (1) reacting long chain ketoacid derivative with hydroxylamine or subjecting ketoacid derivative to an ammoximation to yield oxime derivative; (2) subjecting oxime derivative to Beckmann rearrangement to yield a mixture of mixed amide derivatives; (3) hydrolyzing the mixed amide derivatives to produce long chain ω-amino acid and long chain dibasic acid. 110.-. (canceled)12. The process according to claim 11 , wherein the temperature for oximation is maintained from 0° C. to 100° C. claim 11 , and the pH is in a range of 3 to 14.13. The process according to claim 11 , wherein catalyst for the Beckmann rearrangement of step (2) is sulfuric acid claim 11 , an activated chlorine-containing compound claim 11 , or a mixture of a Lewis acid and an activated chlorine-containing compound.14. The process according to claim 11 , wherein the solvent for oximation claim 11 , ammoximation claim 11 , and Beckmann rearrangement is the same or a different solvent.15. The process according to claim 11 , wherein the product of the Beckmann rearrangement of (II) is a mixture of amide derivative (IIIa) and (IIIb).16. The process according to claim 11 , wherein the mixed amide derivatives are hydrolyzed by an acid or a mixture of acids to produce long chain ω-amino acid (V) and long chain dibasic acid (IV).17. The process according to claim 11 , wherein the mixed amide derivatives are hydrolyzed by a base or a mixture of bases to produce long chain ω-amino acid (V) and long chain dibasic acid (IV).18. The process according to claim 11 , wherein long chain ω-amino acid (V) and long chain dibasic acid (IV) are separated from their mixture by a stepwise neutralization.19. The process according to claim 11 , wherein long chain ω-amino acids of the formula (V) are 9-aminononanoic acid claim 11 , 11-aminoundecanoic acid claim 11 , and 13-aminotridecanoic acid.20. The process ...

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17-01-2019 дата публикации

TRIFLUOROMETHOXYLATION OF ARENES VIA INTRAMOLECULAR TRIFLUOROMETHOXY GROUP MIGRATION

Номер: US20190016670A1

The present invention provides a process of producing a trifluoromethoxylated aryl or trifluoromethoxylated heteroaryl having the structure: 19-. (canceled)11. The process of claim 10 , wherein the second suitable solvent is chloroform claim 10 , dichloromethane claim 10 , nitromethane claim 10 , dimethylforamide claim 10 , diethyl ether claim 10 , tetrahydrofuran claim 10 , dioxane claim 10 , dichloroethane claim 10 , or hexane.12. The process of claim 10 , wherein step (b) is carried out at room temperature.13. The process of claim 10 , wherein step (b) is carried out at a temperature of 50-140° C.14. The process of claim 10 , wherein the compound is maintained in the second suitable solvent for 10-50 hours.15. The process of claim 10 , wherein A is a phenyl or pyridine.16. The process of claim 10 , wherein A is a furan claim 10 , thiophene claim 10 , pyrrole claim 10 , thiazole claim 10 , imidazole claim 10 , pyrazole claim 10 , isooxazole claim 10 , isothiazole claim 10 , naphthalene claim 10 , anthracene claim 10 , pyrimidine claim 10 , pyrazine claim 10 , pyridazine claim 10 , indole claim 10 , indoline claim 10 , benzofuran claim 10 , benzothiophene claim 10 , or quinolone.2037-. (canceled) This application claims priority of U.S. Provisional Application Nos. 62/192,789, filed Jul. 15, 2015; 62/192,462, filed Jul. 14, 2015; 62/063,246, filed Oct. 13, 2014; and 62/062,508, filed Oct. 10, 2014, the contents of each of which are hereby incorporated by reference.Throughout this application various publications are referenced. The disclosures of these documents in their entireties are hereby incorporated by reference into this application in order to more fully describe the state of the art to which this invention pertains.Fluorine atoms are often introduced into organic molecules to enhance their pharmacological properties such as solubility, metabolic and oxidative stability, lipophilicity, and bioavailability. Among the fluorine containing functional groups, ...

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21-01-2021 дата публикации

PROCESS FOR MAKING SARECYCLINE HYDROCHLORIDE

Номер: US20210017123A1
Принадлежит:

The described invention relates to sarecycline, related compounds, intermediates and salts thereof and processes for preparing the same. 2. The process according to claim 1 , wherein step (a) further comprisesi. isopropanol; orii. tetrahydrofuran (THF); oriii. isopropanol and tetrahydrofuran (THF).3. The process according to claim 1 , wherein step (b) further comprises{'sub': '2', 'i. cellulose or SiO; or'}{'sub': 2', '3, 'ii. sodium carbonate (NaCO); or'}iii. water; or{'sub': 2', '4, 'iv. sulfuric acid (HSO); or'}v. ethanol (EtOH); orvi. a combination thereof.4. The process according to claim 1 , wherein step (c) further comprises methanol (MeOH).5. The process according to claim 1 , wherein step (d) further comprises{'sub': '2', 'i. cellulose or SiO; or'}ii. dichloromethane (DCM); oriii. water; oriv. methanol (MeOH); orv. acetone; orvi. a combination thereof.6. The process according to claim 1 , wherein step (e) further comprisesi. ethanol (EtOH); orii. water; oriii. hydrochloric acid (HCl); oriv. a combination thereof.7. The process according to claim 1 , wherein step (d) is repeated at least one time.9. The process according to claim 8 , wherein step (d′) further comprisesi. water; orii. isopropanol; oriii. water and isopropanol.10. The process according to claim 8 , wherein steps (d′) and (d) are repeated at least one time.12. The sarecycline hydrochloride according to claim 11 , wherein the impurity is selected from the group consisting of sancycline claim 11 , 9-sarecycline claim 11 , 7-formylsancycline claim 11 , 7 claim 11 ,9-sarecycline claim 11 , 4R-sarecycline claim 11 , 7-methoxyiminomethylsancycline claim 11 , and a combination thereof.13. The sarecycline hydrochloride according to claim 12 , wherein the sancycline is ≤1.0% (w/w %).14. The sarecycline hydrochloride according to claim 12 , wherein the 9-sarecycline is ≤1.0% (w/w %).15. The sarecycline hydrochloride according to claim 12 , wherein the 7-formylsancycline ≤1.0% (area %).16. The sarecycline ...

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21-01-2021 дата публикации

THICKENING STABILIZER AND SOLVENT COMPOSITION USING SAME FOR PRODUCING ELECTRONIC DEVICE

Номер: US20210017124A1
Принадлежит:

Provided is a compound that thickens a fluid organic material to a desired viscosity and uniformly stabilizes composition thereof. A compound of the present invention is represented by Formula (1): where Rrepresents a monovalent linear aliphatic hydrocarbon group having from 10 to 25 carbons; Rand Rare the same or different, representing a divalent aliphatic hydrocarbon group having 2, 4, 6, or 8 carbons, a divalent alicyclic hydrocarbon group having 6 carbons, or a divalent aromatic hydrocarbon group; Rrepresents a divalent aliphatic hydrocarbon group having from 1 to 8 carbon(s); Rand Rare the same or different, representing a monovalent aliphatic hydrocarbon group having from 1 to 3 carbon(s) or a hydroxyalkylether group Lto Lrepresent an amide bond; in a case where Land Lare —CONH—, Lis —NHCO—, and in a case where Land Lare —NHCO—, Lis —CONH—. 5. A solvent composition for producing an electronic device claim 1 , the solvent composition comprising a miscible material of the composition according to and a fluid organic material.6. The solvent composition for producing an electronic device according to claim 5 , wherein the fluid organic material is at least one selected from a hydrocarbon oil claim 5 , an ether claim 5 , a halogenated hydrocarbon claim 5 , a petroleum component claim 5 , an animal and vegetable oil claim 5 , a silicone oil claim 5 , an ester claim 5 , an aromatic carboxylic acid claim 5 , pyridine claim 5 , and an alcohol. The present invention relates to a novel compound for thickening and stabilizing a fluid organic material such as oil, and a solvent composition containing the compound for producing an electronic device. The present application claims priority to the Japanese Patent Application No. 2018-069615 filed on Mar. 30, 2018, the content of which is hereby incorporated herein.Methods of thickening and stabilizing liquids are industrially very important techniques. For example, mayonnaise and salad dressing, which are emulsions in ...

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26-01-2017 дата публикации

Catalysts and Related Processes For Producing Optically Pure Beta-Lactones From Aldehydes and Compositions Produced Thereby

Номер: US20170021343A1
Автор: Lin Yun-Ming
Принадлежит: The University of Toledo

Bi-functional cobalt-containing catalysts useful for making stereospecific compounds and compositions, along with methods of making, and uses thereof in the syntheses of optically pure β-lactones from aldehydes and ketene are described. Precursors, intermediates, compositions, and particular features of the use if the compositions, such as high enantiomeric selectivity, high yield and low mole percent of catalyst useful are provided. 2. The method of claim 1 , wherein R in structure (11) is selected from: 3-FCH—; 3-ClCH—; 2-ClCH—; 2-FCH—; PhCH—; PhCHCH—; n-CH—; or n-CH—.3. The method of claim 1 , wherein the β-lactone (12) has an enantiomeric excess (ee) greater than or equal to about 70%.4. The method of claim 1 , wherein the β-lactone (12) has an enantiomeric excess (ee) greater than or equal to about 99%.5. A method of producing a β-hydroxy ester comprising using at least one β-lactone (12) produced by the method of .6. A process of enantioselectively producing a β-lactone compound claim 1 , the process comprising:enantioselectively converting ketene into an ammonium enolate using a Lewis acid-Lewis base bi-functional catalyst, anddelivering the ammonium enolate into an aldehyde in the presence of the bi-functional catalyst under conditions sufficient to produce a β-lactone compound;wherein the enantioselective conversion of the aldehyde produces the β-lactone compound in an enantiomeric excess (ee) of at least about 90%.9. A composition of matter comprising a compound of and at least one counterion.10. A composition of matter comprising a compound of claim 8 , wherein:{'sub': 1', '4, 'one of Xthrough Xis O-methyl or vinyl, and the remaining three are hydrogen;'}Y is vinyl;{'sub': 1', '4, 'Rthrough Rare isopropyl or t-butyl; and'}{'sub': 6', '4, 'the composition further comprises at least one counterion selected from the group consisting of: SbF— and BF—.'}11. A composition of matter comprising a compound of claim 8 , wherein:{'sub': 1', '2', '4, 'X, X, and Xare ...

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17-04-2014 дата публикации

TIGECYCLINE CRYSTALLINE HYDRATE AND PREPARATION METHOD THEREFOR AND USE THEREOF

Номер: US20140107357A1
Автор: Hu Lifang
Принадлежит:

Provided are a Tigecycline crystalline hydrate, and a preparation method therefor and use thereof. The crystalline hydrate has high stability for storage, and is used for the manufacture of a medicament for treating or preventing the infection of respiratory system, hepatobiliary system, facial features, urogenital system, bone and joint, skin and soft tissue and endocarditis, septicemia, meningitis caused by susceptible strains of Gram-positive or Gram-negative bacteria, anaerobic bacteria, chlamydia, and mycoplasma in human or animal. 1. A tigecycline crystalline hydrate , characterized in that its molecular formula is CHNO.nHO , n=0.4-4.2. A tigecycline crystalline hydrate according to claim 1 , characterized in being tigecycline.0.5HO hydrate.3. A tigecycline crystalline hydrate according to claim 1 , characterized in being tigecycline.2HO hydrate.4. A tigecycline crystalline hydrate according to claim 1 , characterized in being tigecycline.4HO hydrate.5. A method for the preparation of a tigecycline crystalline hydrate according to claim 1 , characterized in the preparation method comprises the following steps:{'sub': 2', '6', '2', '6', '1', '6', '1', '6', '2', '6', '2', '8', '1', '6', '3', '8', '1', '6', '2', '6', '2', '8', '2', '8', '6', '12, 'method A: the preparation of tigecycline crystalline hydrates direct acylation of 9-aminominocycline with N-tert-butyl acetyl chloride or N-tert-butyl acetic acid 9-amino minocycline disulfate, and sodium hydrogen carbonate or sodium carbonate or potassium carbonate, are suspended in a mixed solvent of 1,3-dimethyl propylidene urea/a lower C-Cnitrile, and a solution of N-tertbutyl acetyl chloride and 1,3-dimethyl propylidene urea/a lower C-Cnitrile is added dropwise at room temperature with stirring; after the addition, the mixture is stirred continuously for 0.3-2 h; after the reaction is completed, a low-molecular C-Calcohol is added to terminate the reaction; the obtained reaction liquor is poured into one or more ...

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17-04-2014 дата публикации

Processes and intermediates for making sweet taste enhancers

Номер: US20140107370A1
Принадлежит: Senomyx Inc

The present invention includes methods/processes and intermediates for preparing compounds having structural Formula (I): wherein X is alkyl, substituted alkyl, alkenyl, substituted alkenyl, heteroalkyl, substituted heteroalkyl, heteroalkenyl, or substituted heteroalkenyl.

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