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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 9194. Отображено 100.
27-02-2010 дата публикации

УСТРОЙСТВО ДЛЯ НИТРОВАНИЯ СПИРТОВ

Номер: RU0000091717U1
Автор: Валешний Сергей Иванович, Валиуллин Камиль Шафикович, Ильин Владимир Петрович, Колганов Евгений Васильевич
Принадлежит: Федеральное государственное унитарное предприятие "Государственный научно-исследовательский институт "Кристалл"

Устройство для нитрования спиртов, отличающееся тем, что оно состоит из двух вертикально расположенных секций, первая секция состоит из вращающейся камеры смешения, выполненной в виде колеса центробежного насоса, между верхним и нижним дисками которого расположены перегородки в виде спиралей, а патрубки подачи смеси спиртов и кислоты введены в полость колеса на меньшем диаметре, причем сливные концы патрубков в полости колеса расположены на минимальном расстоянии друг от друга, вторая секция состоит из камеры смешения, выполненной в виде конического корпуса, снабженного в верхней части кольцевой полостью, в которой концентрично установлена камера смешения первой секции, причем кольцевая полость снабжена отражательным диском, внутренний диаметр которого составляет 0,5÷0,7 диаметра колеса. РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) 91 717 (13) U1 (51) МПК C07C 201/02 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ, ПАТЕНТАМ И ТОВАРНЫМ ЗНАКАМ (12) ОПИСАНИЕ ПОЛЕЗНОЙ МОДЕЛИ К ПАТЕНТУ (21), (22) Заявка: 2009137948/22, 13.10.2009 (24) Дата начала отсчета срока действия патента: 13.10.2009 (45) Опубликовано: 27.02.2010 (73) Патентообладатель(и): Федеральное государственное унитарное предприятие "Государственный научноисследовательский институт "Кристалл" (RU) U 1 9 1 7 1 7 R U Ñòðàíèöà: 1 ru CL U 1 Формула полезной модели Устройство для нитрования спиртов, отличающееся тем, что оно состоит из двух вертикально расположенных секций, первая секция состоит из вращающейся камеры смешения, выполненной в виде колеса центробежного насоса, между верхним и нижним дисками которого расположены перегородки в виде спиралей, а патрубки подачи смеси спиртов и кислоты введены в полость колеса на меньшем диаметре, причем сливные концы патрубков в полости колеса расположены на минимальном расстоянии друг от друга, вторая секция состоит из камеры смешения, выполненной в виде конического корпуса, снабженного в верхней части кольцевой полостью, в которой концентрично установлена камера ...

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Номер записи: 1
27-05-2013 дата публикации

АППАРАТ ДЛЯ ПРОВЕДЕНИЯ ЖИДКОФАЗНЫХ ГЕТЕРОГЕННЫХ ПРОЦЕССОВ

Номер: RU0000128611U1
Автор: Валиуллин Камиль Шафикович, Ильин Владимир Петрович
Принадлежит: Открытое акционерное общество "Государственный научно-исследовательский институт "Кристалл" (ОАО "ГосНИИ "Кристалл")

Аппарат для проведения жидкофазных гетерогенных процессов, содержащий кожухотрубный теплообменник с нижним перетоком, промежуточную емкость, циркуляционную трубу, устройство для смешения и рециркуляции, выполненное в виде колеса осевого насоса, отличающийся тем, что циркуляционная труба дополнительно снабжена кожухотрубным теплообменником, установленным между колесом осевого насоса и нижним перетоком основного теплообменника. 128611 И 1 ко РОССИЙСКАЯ ФЕДЕРАЦИЯ 7 ВУ’? 128 611” 91 ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ИЗВЕЩЕНИЯ К ПАТЕНТУ НА ПОЛЕЗНУЮ МОДЕЛЬ ММ9К Досрочное прекращение действия патента из-за неуплаты в установленный срок пошлины за поддержание патента в силе Дата прекращения действия патента: 18.01.2021 Дата внесения записи в Государственный реестр: 15.10.2021 Дата публикации и номер бюллетеня: 15.10.2021 Бюл. №29 Стр.: 1 ЕЕЭЗсСЬ па ЕП

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Номер записи: 2
17-05-2012 дата публикации

No-Carrier-Added Nucleophilic [F-18] Fluorination of Aromatic Compounds

Номер: US20120123120A1
Автор: Jorge R. Barrio, Nagichettiar Satyamurthy
Принадлежит: UNIVERSITY OF CALIFORNIA

Phenyliodonium ylide derivatives substituted with electron donating as well as electron withdrawing groups on the aromatic ring are shown for use as precursors in aromatic nucleophilic substitution reactions. The iodonium ylide group is substituted by nucleophiles such as halide ions to provide the corresponding haloaryl derivatives. No-carrier-added [F-18]fluoride ion exclusively substitutes the iodonium ylide moiety in these derivatives and provides high specific activity F-18 labeled fluoro derivatives. Protected L-dopa-6-iodonium ylide derivative have been synthesized as a precursors for the preparation of no-carrier-added 6-[F-18]fluoro-L-dopa. The iodonium ylide group in this L-dopa.derivative is nucleophilically substituted by no-carrier-added [F-18]fluoride ion to provide a [F-18]fluoro intermediates which upon acid hydrolysis yielded 6-[F-18]fluoro-L-dopa.

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Номер записи: 3
07-06-2012 дата публикации

Method for synthesis of secondary alcohols

Номер: US20120142934A1
Автор: Chien-Hong Cheng, Jaganathan Karthikeyan, Pang-Chi Huang
Принадлежит: National Tsing Hua University NTHU

A method for synthesis of secondary alcohols is provided for pharmaceutical secondary alcohol by addition of organoboronic acids with aldehydes in presence of the cobalt ion and bidentate ligands as the catalyst. In addition, an enantioselective synthesis method for secondary alcohols is also herein provided in the present invention. The present invention has advantages in using less expensive cobalt ion and commercially available chiral ligands as the catalyst, wide scope of organoboronic acids and aldehydes compatible with this catalytic reaction and achieving excellent yields and/or enantiomeric excess.

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Номер записи: 4
09-08-2012 дата публикации

Method for preparing polyamine compounds

Номер: US20120202934A1
Автор: Asghar Akber Peera, Glenn Nelson Robinson, Ian Anthony Tomlinson
Принадлежит: Angus Chemical Co, Dow Global Technologies LLC

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

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Номер записи: 5
14-02-2013 дата публикации

Process for purifying wastewaters from the workup of crude aromatic nitro compounds

Номер: US20130041189A1
Автор: Bart Van De Voorde, Julia Leschinski, Leo Denissen, Matthias FANKHÄNEL, Petra Deckert, Samuel Neto, Stefan Robert DEIBEL
Принадлежит: BASF SE

The invention relates to a process for purifying crude aromatic nitro compounds which originate from the nitration of aromatic compounds, comprising the single or multiple performance of the following wash stage (a): (a) contacting the crude aromatic nitro compound (N-in) with an aqueous phase (W-res) and then separating the phases to obtain an organic phase (N-res) and an aqueous phase (W-res), wherein at least one demulsifier (D) is present in one or more of the wash stages (a).

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Номер записи: 6
21-03-2013 дата публикации

Process for Making Modulators of Cystic Fibrosis Transmembrane Conductance Regulator

Номер: US20130072522A1
Автор: Adam R. Looker, Bobbianna J. Neubert-Langille, Brian R. Krueger, Dahrika Milfred Yap GUERETTE, Fredrick F. Van Goor, Gregor Zlokarnik, John Demattei, Martin Trudeau, Martyn Curtis Botfield, Michael P. Ryan, Peter Diederik Jan Grootenhuis, Stefanie Roeper
Принадлежит: Vertex Pharmaceuticals Inc

The invention provides a process for the preparation of a compound of Formula 1, comprising coupling a carboxylic acid of Formula 2 with an aniline of Formula 3 in the presence of a coupling agent.

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Номер записи: 7
28-03-2013 дата публикации

Anticancer and Tubulin Polymerisation Inhibition Activity of Benzylidene Indanones and Process of Preparing the Same

Номер: US20130079396A1
Автор: Ajit Kumar Saxena, Arvind Singh Negi, Atul Gupta, Ayyampudur Palanisamy Prakasham, Debabrata Chanda, Suaib Luqman, Tandeep Kaur
Принадлежит: Council of Scientific and Industrial Research CSIR

The present invention relates to benzylidene indanones of general formula 1. The compounds exhibited tubulin polymerisation inhibition. A series of compounds 2-benzylidene 3-(3,4,5-trimethoxyphenyl) indanones having general formulae 1 were synthesized from gallic acid through a chemical process. 2-(3,4-Methylenedioxybenzylidine), 3-(3,4,5-trimethoxyphenyl), 4,5,6-trimethoxyindanone (8), a representative compound of this series possessing the molecular formulae C 29 H 28 O 9 , was synthesized from gallic acid and exhibits potent anticancer activity. Compound 8 was evaluated for acute oral activity in Swiss albino mice and found to be safe up to 300 mg/kg body weight. The anticancer activity of the compounds has been determined, in order to obtain new potent and cost effective molecules using an in vitro cytotoxicity assay.

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Номер записи: 8
11-04-2013 дата публикации

Epoxidation of glycerol and derivatives therefrom

Номер: US20130090497A1
Автор: Andre Pienaar, Laurence Justin Pienaar Wilson, Michael Stockenhuber
Принадлежит: AEL Mining Services Ltd

A method producing a surfactant from glycerol by converting glycerol, in a first step, to glycidol, polymerizing glycidol to an aliphatic alcohol and finally substituting a hydroxyl group with a substitute anion.

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Номер записи: 9
18-04-2013 дата публикации

ASYMMETRIC CYCLIZATION PROCESSES USING UNSATURATED NITRO COMPOUNDS

Номер: US20130096338A1
Автор: Chua Pei Juan, Shi Zugui, Tan Bin, Zhong Guofu
Принадлежит: NANYANG TECHNOLOGICAL UNIVERSITY

Disclosed are processes of forming a compound (33), (35) or (37) 2. The process of claim 1 , further comprising contacting the compound of general formula (23) with a compound of general formula R—X claim 1 , wherein X is one of H claim 1 , halogen claim 1 , —CN claim 1 , —COOR claim 1 , —COSR—COSeRand —CONRRwherein Ris one of halogen claim 1 , —CN claim 1 , an aliphatic claim 1 , an alicyclic claim 1 , an aromatic claim 1 , an arylaliphatic claim 1 , and an arylalicyclic group with a main chain of a length of 1 to about 20 carbon atoms claim 1 , comprising 0 to about 6 heteroatoms selected from the group consisting of N claim 1 , O claim 1 , S claim 1 , Se and Si claim 1 , and Rand Rare independent from one another one of H claim 1 , an aliphatic claim 1 , an alicyclic claim 1 , an aromatic claim 1 , an arylaliphatic claim 1 , and an arylalicyclic group with a main chain of a length of 1 to about 20 carbon atoms claim 1 , comprising 0 to about 6 heteroatoms selected from the group consisting of N claim 1 , O claim 1 , S claim 1 , Se and Si claim 1 , thereby allowing the formation of a compound of general formula (33).3. The process of claim 1 , wherein the compound of general formula (X) is present in a catalytical amount.4. The process of claim 1 , wherein the process is carried out in a solvent.5. The process of claim 1 , wherein contacting the first compound of formula (1) and the second compound of formula (2) is carried out at a temperature selected in the range from about −40° C. to about 40° C.6. The process of claim 5 , wherein contacting the first compound of formula (1) and the second compound of formula (2) is carried out at ambient temperature.923-. (canceled)24. The process of claim 4 , wherein the process is carried out in a polar liquid.25. The process of claim 4 , wherein the process is carried out in a non-polar liquid. This application is a continuation of the U.S. application Ser. No. 12/782,704, filed May 18, 2010, which in turn makes reference ...

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Номер записи: 10
16-05-2013 дата публикации

CARBOCATALYSTS FOR CHEMICAL TRANSFORMATIONS

Номер: US20130123514A1
Автор: Bielawski Christopher W., Dreyer Daniel R., Jia Hong-Peng
Принадлежит: GRAPHEA, INC.

The disclosure relates to catalytically active carbocatalysts, e.g., a graphene oxide or graphite oxide catalyst suitable for use in a variety of chemical transformations. In one embodiment, it relates to a method of catalyzing a chemical reaction of an organic molecule by reacting the organic molecule in the presence of a sufficient amount of graphene oxide or graphite oxide for a time and at a temperature sufficient to allow catalysis of a chemical reaction. According to other embodiments, the reaction may be an oxidation reaction, a hydration reaction, a dehydrogenation reaction, a condensation reaction, or a polymerization reaction. Some reactions may include auto-tandem reactions. The disclosure further provides reaction mixtures containing an organic molecule and graphene oxide or graphite oxide in an amount sufficient to catalyze a reaction of the organic molecule. 1. A method for chemically transforming an organic compound , comprising:(a) contacting the organic compound with a catalytically active carbocatalyst having a surface terminated with one or more peroxide, hydroxyl, aldehyde, or carboxylic acid groups; and(b) transforming the organic compound with the aid of the catalytically active carbocatalyst to form a mixture of a reaction product and a spent or partially spent carbocatalyst.2. The method of claim 1 , wherein the catalytically active carbocatalyst is an oxidized form of graphite.3. The method of claim 2 , wherein the catalytically active carbocatalyst is graphene oxide or graphite oxide.4. The method of claim 1 , wherein the catalytically active carbocatalyst is an oxidized carbon-containing material.5. The method of claim 1 , wherein the catalytically active carbocatalyst is characterized by one or more FT-IR features at about 3150 cm claim 1 ,1685 cm claim 1 , 1280 cm claim 1 , or 1140 cm.629-. (canceled)30. The method of claim 1 , wherein the organic compound has at least one sp-hybridized C—H bond claim 1 , and the transformation involves ...

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Номер записи: 11
23-05-2013 дата публикации

Production of renewable aromatic compounds

Номер: US20130130345A1
Автор: David A. Sikkenga, Wendy Thai, Will SCHROEDER
Принадлежит: JNF BIOCHEMICALS LLC

The invention provides a process for producing a variety renewable aromatic compounds such as benzene, toluene, xylenes, and cumene, as well as compounds derived from these including, for example, aniline, benzoic acid, cresol, cyclohexane, cyclohexanone, phenol and bisphenol A, toluene di-isocyanate, isophthalic acid, phthalic anhydride, terephthalic acid and dimethyl terephthalate. The invention also provides for renewable forms of these aromatic compounds.

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Номер записи: 12
27-06-2013 дата публикации

PROCESS FOR THE PREPARATION OF IODIDES

Номер: US20130165658A1
Автор: Gandelman Mark, Kulbitski Kseniya, Nisnevich Gennady
Принадлежит:

This invention is directed to a process for the preparation of high yield alkyl or aryl iodide from its corresponding carboxylic acid using N-iodo amides. 1. A process for the preparation of iodide , represented by scheme (1):{'br': None, 'R—COOH→R—I\u2003\u2003(1)'}comprising reacting R—COOH with N-iodo amide to yield R—I; wherein R is saturated, linear or branched, substituted or unsubstituted alkyl; substituted or unsubstituted aryl; saturated or unsaturated, substituted or unsubstituted mono- or poly-carbocyclic or heterocyclic ring.2. The process of claim 1 , wherein said amide is carboxamide or sulfonamide.3. The process of claim 1 , wherein said amide is lactame claim 1 , carbamate claim 1 , imide or ureide.4. The process of claim 1 , wherein said amide is 5 claim 1 ,5-dimethylhydantoin claim 1 , 3-benzyl-5 claim 1 ,5-dimethylhydantoin claim 1 , 5-methyl-5-phenylhydantoin claim 1 , 5 claim 1 ,5-diphenylhydantoin claim 1 , 5 claim 1 ,5-hexamethylenehydantoin claim 1 , 5 claim 1 ,5-pentamethylenehydantoin claim 1 , 5 claim 1 ,5-tetramethylenehydantoin claim 1 , succinimide claim 1 , phthalimide claim 1 , saccharine claim 1 , isocyanuric acid claim 1 , 5 claim 1 ,5-dimethylbarbituric acid claim 1 ,-glycoluril claim 1 , 3a claim 1 ,6a-diphenylglycoluril claim 1 , 3a claim 1 ,6a-dimethylglycoluril claim 1 , 4 claim 1 ,4 claim 1 ,5 claim 1 ,5-tetramethyl-2-imidazolidinone claim 1 , 4 claim 1 ,4-dimethyl-2-oxazolidinone or mixture thereof.5. The process of claim 1 , wherein said N-iodo amide is 1 claim 1 ,3-diiodo-5 claim 1 ,5-dimethylhydantoin (DIH) claim 1 , N-iodosuccinimide (NIS) claim 1 , triiodoisocyanuric acid (TICA) claim 1 , 2 claim 1 ,4 claim 1 ,6 claim 1 ,8-tetraiodoglycoluril (TIG) claim 1 , N-iodosaccharine (NISac) claim 1 , or mixture thereof.6. The process of claim 1 , which comprises subjecting the mixture of the R—COOH and N-iodoamide to heat claim 1 , ultrasound claim 1 , or electromagnetic radiation or combination thereof.7. The process of claim 1 ...

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Номер записи: 13
18-07-2013 дата публикации

Isothermal reactor for hydrocarbon nitration

Номер: US20130183206A1
Автор: Daniel M. Trauth
Принадлежит: Angus Chemical Co

Disclosed are a process and an apparatus for synthesizing nitroalkanes by reaction of a hydrocarbon feedstock with aqueous nitric acid. By using an isothermal reactor with multiple input ports for aqueous nitric acid, a hydrocarbon feedstock may be sequentially exposed to a plurality of flows of aqueous nitric acid as it flows through the reactor.

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Номер записи: 14
18-07-2013 дата публикации

METHOD FOR PREPARING 2,3-DIMETHYL-2,3-DINITROBUTANE

Номер: US20130184504A1
Автор: ZHANG Hong, Zhang Shengjian, Zhao Yingxian
Принадлежит: NINGBO INSTITUE OF TECHNOLOGY ZHEJIANG ZHEJIAND

The present invention relates to a method for preparing 2,3-dimethyl-2,3-dinitrobutane (DMNB), which includes the following steps: (1) making titanium-silicate molecular sieve catalyst, acetone, hydrogen peroxide and ammonia contact and react at 65-80° C. to obtain a modified titanium-silicate molecular sieve catalyst; and (2-1) making acetone oxime and hydrogen peroxide contact and react in the presence of the modified titanium-silicate molecular sieve catalyst and water under the conditions of temperature of 60-90° C. and pH of 8-10, and separating DMNB from the reaction products thereof; or (2-2) making acetone, ammonia and hydrogen peroxide contact and react in the presence of the modified titanium-silicate molecular sieve catalyst and water under the conditions of temperature of 60-90° C. and pH of 8-10, and separating DMNB from the reaction products thereof. By the method provided by the present invention, DMNB can be prepared without having to use dangerous chemicals, such as 2-nitropropane, NaH and the like. 1. A method for preparing 2 ,3-dimethyl-2 ,3-dinitrobutane (DMNB) comprising the following steps:(1) making titanium-silicate molecular sieve catalyst, acetone, hydrogen peroxide and ammonia contact and react at 65-80° C. to obtain a modified titanium-silicate molecular sieve catalyst; and(2-1) making acetone oxime and hydrogen peroxide contact and react in the presence of the modified titanium-silicate molecular sieve catalyst and water under the conditions of temperature of 60-90° C. and pH of 8-10, and separating DMNB from the reaction products thereof; or(2-2) making acetone, ammonia and hydrogen peroxide contact and react in the presence of the modified titanium-silicate molecular sieve catalyst and water under the conditions of temperature of 60-90° C. and pH of 8-10, and separating DMNB from the reaction products thereof.2. The method as in claim 1 , wherein in Step (1) claim 1 , the performance for making titanium-silicate molecular sieve ...

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Номер записи: 15
01-08-2013 дата публикации

Organometallic Molybdenum Acetylide Dioxo Complex And Process For The Preparation Thereof

Номер: US20130197245A1
Автор: Acham Vaibhav Ravindrakumar, Biradar Ankush, Dongare Mohan Keraba, Umbarkar Shubhangi Bhalchandra
Принадлежит:

An organometallic molybdenum acetylide dioxo complex of formula (η-CH)MoO(—Cs≡CPh) and provides a simple, short, efficient process for the synthesis of organometallic molybdenum dioxo complex which is used as catalyst for a number of oxidation reactions. 1. Organometallic molybdenum acetylide dioxo complex of formula (η-CH)MoO(—C≡CPh).2. Organometallic molybdenum acetylide dioxo complex as claimed in is useful as catalyst for the oxidation of olefins claim 1 , alcohols claim 1 , anilines claim 1 , sulfides and alkanes.3. Organometallic molybdenum acetylide dioxo complex as claimed in claim 1 , wherein said complex is recyclable.4. Organometallic molybdenum acetylide dioxo complex as claimed in claim 1 , wherein catalytically active species (η-CH) MoO(O)(—C≡CPh) of the said organometallic molybdenum dioxo complex (η-CH) MoO(—C≡CPh) formed after reacting with hydrogen peroxide is water soluble.5. A process for preparation of organometallic molybdenum acetylide dioxo complex of formula (η-CH)MoO(—C≡CPh) as claimed in and the said process comprising the steps of:{'sub': 2', '2', '2, 'i. treating molybdenum trioxide with aqueous halo acids HX wherein X═F, Cl, Br or I in the molar ratio of the trioxide to HX ranging between 1:6 to 1:15 at temperature in the range of 40° C. to 90° C. for period in the range of 2 to 5 hr to obtain aqua complex of dihalo dioxo molybdenum of formula MoOX.2HO wherein X═F, Cl, Br or I;'}{'sub': 2', '2', '2', '2, 'ii. adding dimethylsulphoxide or N,N-dimethylformamide to dihalo dioxo molybdenum as obtained in step (i) in the molar ratio ranging between 1:2 to 1:20 to form greenish adduct of formula MoOX.2DMSO or MoOX.2DMF wherein X═F, Cl, Br or I;'}{'sub': '2', 'iii. treating greenish adduct as obtained in step (ii) with sodium cyclopentadiene in molar ration of 1:1 to 1:20 followed by stirring at the rate of 100 to 1000 rpm to form cyclopentadiene dioxomolybdenum halo complex of formula CpMoOX wherein X═F, Cl, Br or I;'}{'sup': '5', 'sub': 5', ...

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Номер записи: 16
01-08-2013 дата публикации

METHOD FOR PRODUCING NITROBENZENE BY ADIABATIC NITRIDING

Номер: US20130197268A1
Автор: Knauf Thomas, Racoes Alexandre, Rausch Andreas Karl, Wulf Dietrich
Принадлежит: Bayer Intellectual Property GmbH

The invention relates to a process for the continuous production of nitrobenzene by nitration of benzene with a mixture of nitric acid and sulfuric acid under adiabatic conditions, in which unreacted benzene is separated from the crude product obtained after phase separation before washing thereof, using the adiabatic heat of reaction. 19-. (canceled)10. A process for continuously producing nitrobenzene comprisinga) nitrating benzene with a mixture of nitric acid and sulfuric acid under adiabatic conditions to obtain a product;b) separating the product obtained in step a) by phase separation into an aqueous phase comprising sulfuric acid, nitrobenzene, and benzene, and an organic phase comprising nitrobenzene and benzene;c) transferring the aqueous phase obtained in step b) into an evaporator wherein the sulfuric acid is concentrated by pressure reduction, wherein a gaseous stream comprising water, nitrobenzene, and benzene is removed from the evaporator and then condensed, and wherein the resulting concentrated sulfuric acid is fed back into step a);d) separating via distillation from 20% by mass to 100% by mass of the benzene contained in the organic phase obtained in step b) by evaporating the benzene using the adiabatic heat of reaction obtained in step a), wherein a pre-purified nitrobenzene depleted of benzene is obtained;e) washing the pre-purified nitrobenzene obtained in step d) with at least one aqueous phase and subsequently separating the at least one aqueous phase from the nitrobenzene by phase separation to obtain purified nitrobenzene.11. The process of claim 10 , wherein in step d) from 20% by mass to 99.8% by mass of the benzene contained in the organic phase obtained in step b) is separated off and step e) is followed by:f) separating via distillation benzene and water from the purified nitrobenzene obtained in step e) to obtain dried pure nitrobenzene.12. The process of claim 10 , further comprising removing the water from the condensed gaseous ...

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Номер записи: 17
08-08-2013 дата публикации

METHOD FOR CONTINUOUSLY PRODUCING NITROBENZENE

Номер: US20130204043A1
Автор: Knauf Thomas, Lehner Peter, Merkel Michael, Munnig Jurgen, Rausch Andreas Karl
Принадлежит: Bayer Intellectual Property GmbH Creative Campus Monheim

The present invention relates to a continuous process for the production of nitrobenzene by nitration of benzene with nitric acid or mixtures of nitric acid and sulfuric acid to give a crude nitrobenzene, washing of the crude nitrobenzene by means of at least one of each of an acid, alkaline and neutral washing, there being obtained a pre-purified nitrobenzene which, as well as containing nitrobenzene, at least contains also low boilers, optionally middle boilers as well as high boilers and salts, wherein the pre-purified nitrobenzene is purified further by separating off low boilers in a distillation apparatus by evaporation of the low boilers, and separation of nitrobenzene from the resulting further purified nitrobenzene in a distillation apparatus by partial evaporation of nitrobenzene, wherein pure nitrobenzene is removed from the distillation apparatus in gaseous form and is subsequently condensed, and wherein the non-evaporated portion of the further purified nitrobenzene is fed back into the washing at any desired point. 17-. (canceled)8. A process for producing nitrobenzene comprisinga) nitrating benzene with nitric acid or a mixture of nitric acid and sulfuric acid to obtain crude nitrobenzene and subsequently separating excess acid from said crude nitrobenzene;b) washing said crude nitrobenzene from step a) with at least one each of an acid, alkaline, and neutral washing to obtain a mixture comprising pre-purified nitrobenzene and low boilers after the final washing;c) separating the low boilers from the pre-purified nitrobenzene from step b) in a distillation apparatus by evaporation of the low boilers to obtain a bottom product of further purified nitrobenzene depleted of low boilers;d) partially separating nitrobenzene from the further purified nitrobenzene from step c) in a distillation apparatus by partial evaporation of nitrobenzene, wherein pure nitrobenzene is removed from the distillation apparatus in gaseous form and is subsequently condensed; ...

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Номер записи: 18
22-08-2013 дата публикации

Process For Nitroalkane Recovery By Aqueous Phase Recycle To Nitration Reactor

Номер: US20130216443A1
Автор: Pendergast John G., Sawant Mahesh, Trauth Daniel M.
Принадлежит:

Disclosed are a process and an apparatus for synthesizing nitroalkanes by reaction of a hydrocarbon feedstock with aqueous nitric acid. Energy and capital costs may be reduced by recycling a majority of the aqueous phase back to the reactor. 1. An apparatus for synthesizing at least one nitroalkane , the apparatus comprising:a reactor for reacting a hydrocarbon feedstock with aqueous nitric acid to produce a reaction product stream;a cooling system for quenching the reaction product stream such that it phase separates into at least a gas phase, an oil phase, and an aqueous phase;a divider for dividing the aqueous phase into a first aqueous stream and a second aqueous stream;a recycling system for returning the first aqueous stream to the reactor; anda recovery system for recovering the at least one nitroalkane from at least one of the oil phase and the second aqueous stream.2. An apparatus according to claim 1 , wherein the reactor the reactor is a downflow configured reactor.3. An apparatus according to claim 1 , further comprising an absorber for absorbing water-soluble and oil-soluble components from the gas phase into the oil phase and the second aqueous stream to form a gas-recovered mixture. The invention relates to a process for synthesizing nitroalkanes. More specifically, the invention relates to a process for improved nitroalkane recovery in which an aqueous phase is recycled back to the nitration reactor.The nitration of hydrocarbons generally involves the distillation of both an oil phase and an aqueous phase. However, this process requires large energy and capital expenditures.In conventional vapor phase nitration schemes, described in U.S. Pat. Nos. 3,780,115 and 3,869,253, the reactor effluent is rapidly quenched and the quenched mixture is sent to a separator. The gas phase is then withdrawn for purification and recycling and the aqueous phase and the oil phase are separated by decantation and treated simultaneously to recover the desired ...

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Номер записи: 19
22-08-2013 дата публикации

PHOSPHINE LIGANDS FOR CATALYTIC REACTIONS

Номер: US20130217876A1
Автор: BARNES David M., Chan Vincent S., Dunn Travis B., Franczyk Thaddeus S., Haight Anthony R., Shekhar Shashank
Принадлежит: AbbVie Inc.

The disclosure is directed to: (a) phosphacycle ligands; (b) catalyst compositions comprising phosphacycle ligands; and (c) methods of using such phosphacycle ligands and catalyst compositions in bond forming reactions. 2. The phosphine ligand of claim 1 , wherein Vand Vare CR claim 1 , wherein Ris alkoxy.3. The phosphine ligand of claim 1 , wherein Vand Vare CR claim 1 , wherein Ris methoxy.4. The phosphine ligand of claim 1 , wherein Vand Vare CR claim 1 , wherein Ris hydrogen.5. The phosphine ligand of claim 1 , wherein V claim 1 , Vand Vare CR claim 1 , wherein Ris alkyl.6. The phosphine ligand of claim 1 , wherein V claim 1 , Vand Vare CR claim 1 , wherein Ris isopropyl.7. The phosphine ligand of claim 1 , wherein Vand Vare CR claim 1 , wherein Ris hydrogen.10. The phosphine ligand of claim 1 , wherein the ligand is selected from the group consisting of:2,2,6,6-tetramethyl-1-(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphinane;2,2,6,6-tetramethyl-1-(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphinan-4-one;2,2,6,6-tetramethyl-1-(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphinan-4-ol;7,7,9,9-tetramethyl-8-(2′,4′,6′-triisopropylbiphenyl-2-yl)-1,4-dioxa-8-phosphaspiro[4.5]decane;8,8,10,10-tetramethyl-9-(2′,4′,6′-triisopropylbiphenyl-2-yl)-1,5-dioxa-9-phosphaspiro[5.5]undecane;3,3,8,8,10,10-hexamethyl-9-(2′,4′,6′-triisopropylbiphenyl-2-yl)-1,5-dioxa-9-phosphaspiro[5.5]undecane;1-(2′-(dimethylamino)-6′-methoxybiphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(2′,6′-bis(dimethylamino)biphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(2′,6′-dimethoxybiphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(2′,6′-diisopropoxybiphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(2′-(dimethylamino)biphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(biphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(1,1′-binaphthyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(2′-methoxy-1,1′-binaphthyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(3,6-dimethoxybiphenyl-2-yl)-2,2,6,6- ...

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Номер записи: 20
29-08-2013 дата публикации

Fluoroalkylation Methods And Reagents

Номер: US20130225815A1
Автор: Hiroyuki Morimoto, John F. Hartwig, Patrick Fier
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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Номер записи: 21
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
Автор: Kazuo Murakami, Yoshiji Takemoto
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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Номер записи: 22
19-09-2013 дата публикации

Processes for preparing benzimidazole compounds

Номер: US20130245279A1
Автор: Anthony D. Piscopio, Bruno P. Hache, James Gair Ford, John Demattei, John Leonard, Koen Peeters, Matthew Charles Evans, Sagar Shakya, Simon Mark Pointon, Timothy John Lilley
Принадлежит: Array Biopharma Inc, AstraZeneca AB

Provided are processes for the preparation of benzimidazole structures having Formula VIIIb-1: and salts and solvates thereof, wherein Z, X 5 , R 2b , R 2c and R 10 are as defined herein. Compounds of Formula VIIIb-1 are useful for the preparation of benzimidazole derivatives.

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Номер записи: 23
19-09-2013 дата публикации

Apparatus and Process for Using a Nitroalkane as an Entrainer for Azeotropic Removal of Water from Aqueous Acid Solution

Номер: US20130245340A1
Автор: Pendergast John G., Sawant Mahesh Ratnakar, Trauth Daniel M.
Принадлежит:

Disclosed are a process and an apparatus for concentrating an organic acid by using a nitroalkane as an entrainer for the azeotropic removal of water from an aqueous organic acid solution. The nitroalkane may be the same as a nitroalkane that is the product of a high pressure nitration process that produces nitroalkanes and aqueous organic acid. 1. A process comprising:supplying a feed stream to an azeotropic distillation column, wherein the feed stream comprises water and an organic acid;using a nitroalkane as an entrainer in the azeotropic distillation column, such that the feed stream is separated into at least a top stream and a bottom stream, wherein the top stream comprises the nitroalkane and water and wherein the bottom stream comprises the organic acid;separating the top stream into an organic phase and an aqueous phase, the organic phase comprising the nitroalkane; andreturning at least a portion of the organic phase to the azeotropic distillation column.2. A process according to claim 1 , wherein the nitroalkane is selected from the group consisting of 1-nitropropane and 2-nitropropane.3. A process according to claim 1 , wherein the bottom stream is at least 90 weight percent of the organic acid.4. A process according to claim 1 , wherein the azeotropic distillation column comprises at least forty stages.5. A process according to claim 1 , wherein the organic acid is present in the bottom stream in a higher concentration than in the feed stream.6. A process according to claim 1 , further comprising returning at least a portion of the aqueous phase to the azeotropic distillation column.7. A process comprising:reacting a hydrocarbon feedstock with aqueous nitric acid in a reactor to produce a product stream comprising a product nitroalkane and byproducts;degassing the product stream to produce a liquid stream;separating the liquid stream in a stripping apparatus into a first top stream and a first bottom stream, wherein the first top stream comprises the ...

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Номер записи: 24
26-09-2013 дата публикации

POLYMER SUPPORTED REAGENTS AND METHODS OR REDUCING AROMATIC NITRO COMPOUNDS BY USING THE SAME

Номер: US20130253083A1
Автор: Cho Jin, Han Yang-Kyoo, Lee Sang-Mi, Shin Seung-Hoon
Принадлежит:

The present invention relates to a polymer supported reagent comprising a novel crosslinked mesoporous polymer, enabling a simple and easy production of an azoxy compound or an azo compound from an aromatic nitro compound, and a method of selectively reducing an aromatic nitro compound by using the same. The polymer supported reagent comprises a certain acrylamide mesoporous crosslinked polymer. 2. The polymer supported reagent in accordance with claim 1 , wherein the mesoporous crosslinked polymer further comprises at least one polymer repeating unit selected from the group consisting of a styrene repeating unit and a vinyl repeating unit.3. The polymer supported reagent in accordance with claim 1 , wherein the polymer supported reagent has a shape of a spherical particle having a particle size of 20 to 300 μm.4. The polymer supported reagent in accordance with claim 1 , wherein it comprises a plurality of pores having a diameter of 2.0 to 10.0 nm.5. The polymer supported reagent in accordance with claim 1 , wherein the mesoporous crosslinked polymer comprises the repeating unit of Chemical Formula 1 and a styrene repeating unit at a mole ratio of 10:0 to 1:9.6. The polymer supported reagent in accordance with claim 1 , wherein it is used for a reduction reaction of an aromatic nitro compound.8. The method of producing a polymer supported reagent of claim 7 , wherein the monomer composition further comprises at least one monomer selected from the group consisting of a styrene monomer and a vinyl monomer.9. The method of producing a polymer supported reagent of claim 7 , wherein the step of the suspension polymerization comprises the steps of dissolving the crosslinker claim 7 , the radical initiator claim 7 , and the monomer composition in an oil-soluble organic solvent to form an oil-soluble solution; and dispersing the oil-soluble solution in water with a surfactant dissolved therein to carry out the suspension polymerization.10. The method of producing a polymer ...

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Номер записи: 25
24-10-2013 дата публикации

PALLADIUM CATALYST, METHOD FOR ITS PREPARATION AND ITS USE

Номер: US20130281700A1
Автор: DALICZEK Zoltán, FINTA Zoltán, SOÓS Tibor, Timári Géza, Vlád Gábor
Принадлежит:

The invention relates to palladium(0)-tris{tri-[3,5-bis(trifluoromethyl)-phenyl]-phosphine} complex of formula (I), as well as to its preparation and use. 2. The composition of in a solid form.3. The composition of having a melting point of 220° C. as determined by DSC in inert atmosphere.4. The composition of claim 1 , having a decomposition point of 169.5° C. as determined by DSC in air under atmospheric pressure.5. A palladium(0) complex comprising three fluorinated phosphine compounds.6. The palladium(0) complex of exhibiting a stability characterized by no measurable decomposition on the basis of P claim 5 , F claim 5 , C and H NMR spectra following 4 months of storage in air at a temperature of 25° C.7. The palladium(0) complex of exhibiting a stability characterized by no measurable decomposition on the basis of P claim 5 , F claim 5 , C and H NMR spectra following 20 months of storage in air at room temperature.8. The palladium(0) complex of having a melting point in inert atmosphere of 220° C.9. The palladium(0) complex of exhibiting stability at any temperature below its melting point.10. The palladium(0) complex of exhibiting insolubility in water at industrially relevant temperatures and stability when stored in water.11. The palladium(0) complex of comprising a yellow solid.12. The palladium(0) complex of that dissolves at around 90° C. in aqueous alcohols.13. The palladium(0) complex of having catalytic activity in cross coupling reactions at a concentration of from 0.1 to 0.3 mole % of the substrate.14. A method for catalysing a C—C claim 5 , C-heteroatom claim 5 , or hydrogenation reaction comprising carrying out the C—C claim 5 , C-heteroatom or hydrogenation reaction in the presence of the palladium(0) complex of .15. The method of claim 14 , wherein the reaction is a C—C cross-coupling reaction.16. The method of claim 14 , wherein the C—C cross-coupling reaction is selected from the group consisting of: Suzuki coupling claim 14 , Heck coupling and ...

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Номер записи: 26
31-10-2013 дата публикации

Methods for the synthesis of activated ethylfumarates and their use as intermediates

Номер: US20130289278A1
Автор: Freeman John J., IV Otto, Kaur Navneet, Kraft Kelly Sullivan, Pavia Vinnie, Phanstiel, Serwinski Paul
Принадлежит: MANNKIND CORP

Disclosed embodiments relate to improved methods for the synthesis of activated fumarate intermediates and their use in chemical synthesis. Disclosed embodiments describe the synthesis of activated fumarate esters including those derived from activating groups including: 4-nitrophenyl, diphenylphosphoryl azide, pivaloyl chloride, chlorosulfonyl isocyanate, p-nitrophenol, MEF, trifluoroacetyl and chlorine, for example, ethyl fumaroyl chloride and the subsequent use of the activated ester in situ. Further embodiments describe the improved synthesis of substituted aminoalkyl-diketopiperazines from unisolated and unpurified intermediates allowing for improved yields and reactor throughput. 2. The method of further comprising the step of removing a protecting group from the aminoalkyl-diketopiperazine prior to reaction with the activated monoethyl fumarate.3. The method of wherein the activated derivative is a 4-nitrophenyl ester.4. The method of wherein the activated derivative is a mixed anhydride resulting from the reaction of monoethyl fumarate and a reagent selected from the group comprising: diphenylphosphoryl azide claim 1 , pivaloyl chloride claim 1 , chlorosulfonyl isocyanate claim 1 , and trifluoroacetic anhydride.5. The method of wherein the activated derivative is a mixed anhydride generated by reacting monoethyl fumaroyl chloride with pivalic acid.6. The method of further comprising saponification of the ethyl esters of the diketopiperazine of Formula 1.7. The method of further comprising isolation of the activated derivative of monoethyl fumarate before reacting with the aminoalkyldiketopiperazine.8. A method for the synthesis of an activated 4-nitrophenyl ester of mono-ethyl fumarate comprising:in a first reaction mixture, providing a reactive electrophilic derivative of monoethyl fumaric acid;in a second reaction mixture, generating the salt of 4-nitrophenol by reacting with an appropriate base chosen from the group comprising: organic and inorganic ...

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Номер записи: 27
09-01-2014 дата публикации

New palladium catalyst, method for its preparation and its use

Номер: US20140012004A1
Автор: Gábor Vlád, Géza Timári, Tibor SOÓS, Zoltán DALICZEK, Zoltán Finta
Принадлежит: H4SEP KFT

The invention relates to palladium(0) tris{tri-[3,5-bis(trifluoromethyl)-phenyl]-phosphine} complex of formula (I), as well as to its preparation and use. This compound is outstandingly stable, and can be used as catalyst with excellent results.

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Номер записи: 28
30-01-2014 дата публикации

Ether-based reactive plasticizer for plastic bonded explosives

Номер: US20140031593A1
Автор: Bum Jae Lee, In Joo Bae, Jin Seuk Kim, Young Hwan Kwon
Принадлежит: Agency for Defence Development

Disclosed is an energetic reactive plasticizer for a plastic bonded explosive (PBX), and specifically an energetic reactive plasticizer for PBX which has high performance and insensitiveness without a plasticizer leak by being bonded with a polymer binder for a plastic bonded explosive.

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Номер записи: 29
06-02-2014 дата публикации

Compositions and processes of preparing and using the same

Номер: US20140039182A1
Автор: Changho HAN, David A. Colby, Mark V. RIOFSKI
Принадлежит: PURDUE RESEARCH FOUNDATION

The present invention relates to compositions, for example, the DBU/Hexafluoroacetone hydrate salt, and processes of preparing and using the same for the modification of chemical compounds via the release of trifluoroacetate. The DBU/Hexafluoroacetone hydrate salt can perform trifluoromethylation reactions on chemical compounds, such as carbonyl group-containing compounds.

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Номер записи: 30
20-02-2014 дата публикации

Modulators of atp-binding cassette transporters

Номер: US20140051724A1
Автор: Anna Hazlewood, Ashvani Singh, Fredrick Van Goor, Jason Mccartney, Jinglan Zhou, Peter Grootenhuis, Sara Hadida-Ruah
Принадлежит: Vertex Pharmaceuticals Inc

The present invention relates to modulators of ATP-Binding Cassette (“ABC”) transporters or fragments thereof, including Cystic Fibrosis Transmembrane Conductance Regulator, compositions thereof, and methods therewith. The present invention also relates to methods of treating ABC transporter mediated diseases using such modulators.

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Номер записи: 31
20-02-2014 дата публикации

METHOD FOR PRODUCING FIVE-MEMBERED RING-CONTAINING COMPOUND

Номер: US20140051874A1
Автор: Hayashi Yujiro
Принадлежит: ONO PHARMACEUTICAL CO., LTD.

The present invention provides a method that allows production of stereospecific and asymmetrical five-membered ring-containing compounds serving as synthetic intermediates for formation of five-membered rings of prostaglandins and the like, with high yield and excellent stereoselectivity in terms of diastereoselectivity and enantioselectivity in a short process without requiring troublesome procedures such as optical resolution. The method for producing a five-membered ring-containing compound includes a cyclization step of condensing and cyclizing an α,β-unsaturated nitro compound represented by the following chemical formula (I) with a 1,4-butanedione compound, in the presence of a catalyst formed by a compound having a pyrrolidine ring and an optically active α-carbon relative to the nitrogen on the ring, in a water-insoluble organic solvent and/or a non-oxygen atom-containing water-soluble organic solvent so as to produce the five-membered ring-containing compound represented by the following chemical formula (II). 2. The method for producing a five-membered ring-containing compound according to claim 1 , further comprising claim 1 , after the cyclization step claim 1 , a reduction step of reducing claim 1 , with a reducing agent claim 1 , the Athat is the aldehyde group to the hydroxymethyl group.6. The method for producing a five-membered ring-containing compound according to claim 1 , wherein the water-insoluble organic solvent is at least one selected from a halogen-containing organic solvent claim 1 , an aromatic organic solvent claim 1 , a hydrocarbon organic solvent and an acyclic ether organic solvent claim 1 , and the non-oxygen atom-containing water-soluble organic solvent is a nitrile-substituted hydrocarbon organic solvent.7. The method for producing a five-membered ring-containing compound according to claim 6 , wherein the water-insoluble organic solvent is the halogen-containing organic solvent selected from dichloromethane claim 6 , ...

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Номер записи: 32
27-02-2014 дата публикации

New Cyclopentadienyl, Indenyl or Fluorenyl Substituted Phosphine Compounds and Their Use in Catalytic Reactions

Номер: US20140058101A1
Автор: Almena Juan, Fleckenstein Christoph, Kadyrov Renat, Monsees Axel, Plenio Herbert, Riermeier Thomas
Принадлежит: EVONIK DEGUSSA GmbH

The invention is directed to a phosphine compound represented by general formula (1) wherein R′ and R″ independently are selected from alkyl, cycloalkyl and 2-furyl radicals, or R′ and R″ are joined together to form with the phosphorous atom a carbon-phosphorous monocycle comprising at least 3 carbon atoms or a carbon-phosphorous bicycle; the alkyl radicals, cycloalkyl radicals, and carbon-phosphorous monocycle being unsubstituted or substituted by at least one radical selected from the group of alkyl, cycloalkyl, aryl, alkoxy, and aryloxy radicals; Cpis a partially substituted or completely substituted cyclopentadien-1-yl group, including substitutions resulting in a fused ring system, and wherein a substitution at the 1-position of the cyclopentadien-1-yl group is mandatory when the cyclopentadien-1-yl group is not part of a fused ring system or is part of an indenyl group. Also claimed is the use of these phosphines as ligands in catalytic reactions and the preparation of these phosphines. 160-. (canceled)62. The method according to claim 61 , wherein the phosphine compound or the phosphonium salt is used in combination with the transition metal as a coordination compound.63. The method according to claim 61 , wherein the preparation of the organic compound includes the formation of a C—C bond or C-heteroatom bond.64. The method according to claim 61 , wherein the transition metal is Pd and the preparation of the organic compound includes the formation of a C—C bond and a reaction selected from the group consisting of:Suzuki cross-coupling of organoboron compounds with aryl, heteroaryl or vinyl halides or pseudohalides;Stille cross-coupling of organotin compounds with carbon electrophiles comprising a halogen or pseudohalogen as leaving group;Hiyama cross-coupling of organosilanes with aryl, heteroaryl or vinyl halides or pseudohalides;Negishi cross-coupling of organozinc compounds with aryl, heteroaryl or vinyl halides or pseudohalides;Kumada cross-coupling of ...

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Номер записи: 33
06-03-2014 дата публикации

PROCESS FOR PREPARING 6-IODO-2-OXINDOLE

Номер: US20140066634A1
Автор: Bao Yuhui, Huang Yao, Lu Jun, SHI Wenjian, Song Yanli, Weber Dirk
Принадлежит: BOEHRINGER INGELHEIM INTERNATIONAL GMBH

Disclosed is a method for the synthesis of 6-iodo-2-oxindole useful as intermediate in the manufacture of pharmaceutically active ingredients. Also disclosed is a novel intermediate used in the synthesis of this compound. 2. The method according to claim 1 , wherein a suitable base is sodium methanolate or sodium ethanolate.3. The method according to claim 1 , wherein the reaction is conducted in a suitable solvent or mixture of solvents.5. The method according to claim 4 , wherein a suitable reducing agent in a) is a tin(II)-based reducing agent.6. The method according to claim 4 , wherein the reduction reaction in a) is conducted in a suitable solvent or mixture of solvents.7. The method according to claim 4 , wherein a suitable acid in b) is aqueous HCl.8. The method according to claim 4 , wherein the cyclization and/or decarboxylation and/or further reduction reaction in b) is conducted in a suitable solvent or mixture of solvents.9. The method according to claim 1 , wherein the intermediate compound of formula (B) is isolated.10. The method according to claim 1 , wherein the intermediate compound obtained from step a) of is isolated.11. The method according to claim 4 , wherein the intermediate compound obtained from any reactions of step b) of aspect 4 is isolated.12. The method according to claim 4 , wherein the intermediate compound of formula (B) and/or the intermediate compound obtained from step a) of is/are isolated.13. The method according to claim 1 , wherein R and R′ are the same and are ethyl or methyl.14. The method according to claim 1 , wherein the compound of formula (A) is prepared by iodination of 2-chloro-nitrobenzene.15. The method according to claim 14 , wherein the system I/NalOis used for iodination.16. The method according to claim 14 , wherein the reaction is conducted in a suitable solvent or mixture of solvents. This invention relates to a novel method for the synthesis of 6-iodo-2-oxindole useful as intermediate in the manufacture of ...

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Номер записи: 34
06-03-2014 дата публикации

PROCESS FOR THE PREPARATION OF BRONOPOL

Номер: US20140066662A1
Автор: OREN Jacob
Принадлежит:

The invention provides a process for preparing bronopol, which process comprises charging a reaction vessel with water, bromopicrin, nitromethane and paraformaldehyde, gradually feeding a base into said reaction vessel under stirring, bringing the reaction to completion and separating bronopol from the aqueous reaction mixture. 1) A process for preparing bronopol , which process comprises charging a reaction vessel with water , bromopicrin , nitromethane and paraformaldehyde , gradually feeding a base into said reaction vessel under stirring , bringing the reaction to completion and separating bronopol from the aqueous reaction mixture.2) A process according to wherein the molar ratio between the total amount of the base fed into the reaction vessel and the bromopicrin is in the range of 1:100-10:100.3) A process according to claim 2 , wherein the base to bromopicrin ratio is in the range between 3:100 and 7:100.4) A process according to any one of the preceding claims claim 2 , wherein the base is fed to the reaction vessel in the form of an aqueous solution claim 2 , in which the concentration of the base is between 0.1 and 1.25N.5) A process according to claim 4 , wherein the base is provided as an aqueous solution with a concentration between 0.2 and 0.5N.6) A process according to claim 5 , wherein an aqueous solution of sodium hydroxide with a weight concentration in the range between 0.8 and 2% is used.7) A process according to any one of the preceding claim claim 1 , claim 1 , wherein at least a portion of the base is fed while the temperature in the reaction mixture is above 41° C.8) A process according to claim 7 , wherein at least 30% of the total amount of the base is fed to the reaction mixture at a temperature in the range between 45 and 60° C.9) A process for preparing bronopol claim 7 , which process comprises charging a reaction vessel with water claim 7 , bromopicrin claim 7 , nitromethane and formaldehyde source claim 7 , gradually feeding a base ...

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Номер записи: 35
03-04-2014 дата публикации

Process for producing ester compound

Номер: US20140094616A1
Автор: Leopold Mpaka LUTETE, Tetsuya Ikemoto, Toshiaki Aikawa
Принадлежит: Sumitomo Chemical Co Ltd

Compound (1) or a salt that is useful as an intermediate for the production of a medicine, an agrochemical or the like can be produced by a process including the following steps: (A) reacting an aldehyde (2) with nitromethane to produce a nitroaldehyde; (B) reacting the nitroaldehyde with an alcohol to produce a nitroacetal; (C) reducing the nitroacetal to produce an aminoacetal; (D) protecting an amino group in the aminoacetal to produce a protected aminoacetal; (E) treating the protected aminoacetal with an acid and subsequently with a base and then reacting the resultant product with a cyanating agent to produce a nitrile; (F) hydrolyzing the nitrile to produce a protected amino acid; and (G) substituting a group R 5 in the protected amino acid by a hydrogen atom and protecting a carboxyl group therein.

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Номер записи: 36
07-01-2021 дата публикации

PROCESS FOR PRODUCTION OF GLYCOPYRRONIUM TOSYLATE

Номер: US20210002219A1
Автор: Molteni Renato, SHAW Anthony Adrian, Vigano Enrico
Принадлежит:

Provided herein are methods for the production of glycopyrronium tosylate and glycopyrronium tosylate compositions. Also provided herein are compositions useful in the production of glycopyrronium tosylate. Additionally provided herein are glycopyrronium tosylate compositions. Glycopyrronium tosylate is useful for the treatment of, among other conditions, hyperhidrosis. 119-. (canceled)20. A glycopyrrolate base composition comprising threo-glycopyrrolate base and erythro-glycopyrrolate base , wherein the threo-glycopyrrolate base is at least 95% of the total glycopyrrolate base content of the composition and the erythro-glycopyrrolate base is less than 5% of the total glycopyrrolate base content of the composition.21. The glycopyrrolate base composition of claim 20 , wherein the threo-glycopyrrolate base is at least 96% of the total glycopyrrolate base content of the composition and the erythro-glycopyrrolate base is less than 4% of the total glycopyrrolate base content of the composition.22. The glycopyrrolate base composition of claim 20 , wherein the threo-glycopyrrolate base is at least 97% of the total glycopyrrolate base content of the composition and the erythro-glycopyrrolate base is less than 3% of the total glycopyrrolate base content of the composition.24. A glycopyrronium tosylate composition comprising threo-glycopyrronium tosylate and erythro-glycopyrronium tosylate claim 20 , wherein the threo glycopyrronium tosylate is at least 95% of the total glycopyrrolate tosylate content of the composition and the erythro-glycopyrronium tosylate is less than 5% of the total glycopyrronium tosylate content of the composition.25. The glycopyrronium tosylate composition of claim 24 , wherein the threo-glycopyrronium tosylate is at least 96% of the total glycopyrronium tosylate content of the composition and the erythro-glycopyrronium tosylate is less than 4% of the total glycopyrronium tosylate content of the composition.26. The glycopyrronium tosylate composition ...

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Номер записи: 37
03-01-2019 дата публикации

Organic functional compound for preparing organic electronic device and application thereof

Номер: US20190006609A1
Автор: Junyou Pan, XI Yang
Принадлежит: Guangzhou Chinaray Optoelectronic Materials Ltd

The present invention discloses an organic functional compound for preparing an organic electronic device and an application thereof. The organic functional compound has a general formula (I). The organic functional compound comprises an organic functional group and a solubilizing group, thereby imparting a good solubility and film-forming ability. The organic functional compound also excels in maintaining the performance of the functional group in a device. The organic functional compound and a composition or mixture comprising the organic functional compound have a good printability and film-forming ability, facilitating solution-processing, particularly in printing techniques, and obtaining a high-performance small-molecule organic electronic device, particularly an organic electroluminescent device. FSG] k   (I)

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Номер записи: 38
27-01-2022 дата публикации

Process for the preparation of latanoprostene bunod and intermediate thereof and compositions comprising the same

Номер: US20220024849A1
Автор: Ming-Kun Hsu, Shih-Yi Wei, Tzyh-Mann Wei
Принадлежит: Chirogate International Inc

Processes for preparing latanoprostene bunod and an intermediate prepared from the process. Also latanoprostene bunod compositions having high-purity latanoprostene bunod.

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Номер записи: 39
27-01-2022 дата публикации

METHOD FOR PREPARING 2-ETHYL-4-FLUORO-1-NITROBENZENE

Номер: US20220024850A1
Автор: CHEN Lihuang, Liu Yang, Wu Yong, XUE Duoqing, ZHAI Lianhua
Принадлежит:

The present disclosure provides a method for preparing 2-ethyl-4-fluoro-1-nitrobenzene, including: (1) nitrifying 3-fluoroacetophenone with a nitration reagent, to obtain 1-(5-fluoro-2-nitrophenyl)ethanone; (2) reducing 1-(5-fluoro-2-nitrophenyl)ethanone with a reducing agent, to obtain 4-fluoro-2-(1-hydroxyethyl)-1-nitrobenzene; (3) iodinating 4-fluoro-2-(1-hydroxyethyl)-1-nitrobenzene, to obtain 4-fluoro-2-(1-iodoethyl)-1-nitrobenzene; and (4) reducing 4-fluoro-2-(1-iodoethyl)-1-nitrobenzene with a reducing agent, to obtain 2-ethyl-4-fluoro-1-nitrobenzene. 2. The method as claimed in claim 1 , wherein the nitration reagent in step (1) is fuming nitric acid claim 1 , and a mass ratio of the fuming nitric acid to 3-fluoroacetophenone is in the range of (5.0-8.0):1.3. The method as claimed in or claim 1 , wherein the nitrifying in step (1) is performed at a temperature of −15° C. to −5° C. for 2-5 h.4. The method as claimed in claim 1 , wherein step (1) further comprises subjecting a nitrified solution obtained after nitrifying 3-fluoroacetophenone to a post-treatment;the post-treatment comprises: quenching the nitrified solution with ice water, stirring and filtering the nitrified solution, to obtain a solid phase, and collecting the solid phase, to obtain 1-(5-fluoro-2-nitrophenyl)ethanone, wherein the stirring is performed at a temperature of 0° C. to 5° C. for 30-90 min.5. The method as claimed in claim 1 , wherein the reducing agent used in step (2) is sodium borohydride claim 1 , and a molar ratio of sodium borohydride to 1-(5-fluoro-2-nitrophenyl)ethanone is in the range of (0.3-2.0):1.6. The method as claimed in claim 1 , wherein the reducing in step (2) is performed at a temperature of 15° C. to 25° C. for 1-3 h.7. The method as claimed in claim 1 , wherein the reducing in step (2) is performed in the presence of a solvent;the solvent is tetrahydrofuran and/or absolute methanol, andthe solvent is used in an amount of 0.8-1.5 L, based on 1 mol of 1-(5-fluoro- ...

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Номер записи: 40
10-01-2019 дата публикации

Methods for the synthesis of activated ethylfumarates and their use as intermediates

Номер: US20190010131A1
Автор: Freeman John J., Kaur Navneet, Kraft Kelly Sullivan, Pavia Vincent, Phanstiel Otto, Serwinski Paul
Принадлежит:

Disclosed embodiments relate to improved methods for the synthesis of activated fumarate intermediates and their use in chemical synthesis. Disclosed embodiments describe the synthesis of activated fumarate esters including those derived from activating groups including: 4-nitrophenyl, diphenylphophoryl azide, pivaloyl chloride, chlorosulfonyl isocyanate, p-nitrophenol, MEF, trifluoroacetyl and chlorine, for example, ethyl fumaroyl chloride and the subsequent use of the activated ester in situ. Further embodiments describe the improved synthesis of substituted aminoalkyl-diketopiperazines from unisolated and unpurified intermediates allowing for improved yields and reactor throughput. 2. The method of claim 1 , wherein the organic solvent is selected from acetone claim 1 , acetonitrile claim 1 , ethyl acetate claim 1 , tetrahydrofuran claim 1 , and dichloromethane.3. The method of claim 1 , wherein the inorganic metallic base is selected from sodium carbonate and sodium hydroxide.4. The method of claim 1 , wherein the base is provided in an amount of 1 to 2 equivalents based on the amount of 4-nitrophenol.5. The method of claim 1 , wherein the ethyl fumaryl chloride is provided in an amount of 0.5 to 2 equivalents based on the amount of 4-nitrophenol.6. The method of claim 1 , wherein the inorganic metallic base is added as an aqueous mixture to a solution of 4-nitrophenol in the organic solvent.7. The method of claim 1 , wherein the ethyl fumaryl chloride is added to a mixture of 4-nitrophenol and the inorganic metallic base claim 1 , with cooling.8. The method of claim 1 , wherein the aminoalkyl-diketopiperazine is mixed with an organic solvent to form an aminoalkyl-diketopiperazine-containing mixture prior to adding the aminoalkyl-diketopiperazine.9. The method of claim 8 , wherein the organic solvent in the aminoalkyl-diketopiperazine-containing mixture is the same organic solvent used to form the mono-ethyl fumarate ester.10. The method of claim 8 , wherein the ...

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Номер записи: 41
18-01-2018 дата публикации

PROCESS FOR THE PREPARATION OF BENZONORBORNENES

Номер: US20180016211A1
Автор: ANTELMANN Bjorn, BOIS Fanny, DE MESMAEKER Alain, Gribkov Denis, Walter Harald
Принадлежит: SYNGENTA CROP PROTECTION, LLC

The present invention relates to a novel a process for the preparation of 9-dichloromethylene-1,2,3,4-tetrahydro-1,4-methano-naphthalen-5-ylamine which process comprises a) reacting cyclopentadiene in the presence of a radical initiator and CXCl3, wherein X is chloro or bromo, to a compound of formula II, or aa) reacting cyclopentadiene with CXCl3, wherein X is chloro, in the presence of a metal catalyst to a compound of formula II, wherein X is chloro, b) reacting the compound of formula II with a base in the presence of an appropriate solvent to the compound of formula III, c) and converting the compound of formula III in the presence of 1,2-dehydro-6-nitrobenzene to the compound of formula IV, and d) hydrogenating the compound of formula IV in the presence of a metal catalyst. 1. A compound of formula IV This application is a divisional of U.S. patent application Ser. No. 14/603857, filed Jan. 23, 2015 which is a divisional of U.S. patent application Ser. No. 13/126380 filed Apr. 27, 2011, now patented as U.S. Pat. No. 9,115,043 issued Aug. 25, 2015, which was a 371 application of International Application No. PCT/EP2009/062525, filed Sep. 28, 2009, which claims priority to EP Patent Application 08018721.4, filed Oct. 27, 2008, and EP Patent Application No. 09161388.5 filed May 28, 2009, the contents of which are incorporated herein by reference herein.The present invention relates to the preparation of 9-dichloromethylene-1,2,3,4-tetrahydro-1, 4-methano-naphthalen-5-ylamine.The compound 9-dichloromethylene-1,2,3,4-tetrahydro-1,4-methano-naphthalen-5-ylamine is a valuable intermediate for the preparation of benzonorbornene fungicides, as described for example in WO 2007/048556.It is known from WO 2007/048556 to prepare 9-dichloromethylene-1,2,3,4-tetrahydro-1, 4-methano-naphthalen-5-ylamine bya) reacting the compound of formula Ain the presence of an alkyl nitrite with a compound of formula Bwherein R′ and R″ are e.g. C-Calkyl, to a compound of formula Cb) ...

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Номер записи: 42
16-01-2020 дата публикации

METHOD FOR PRODUCING NITROBENZENE

Номер: US20200017434A1
Автор: Chan Denise, Knauf Thomas, Muennig Juergen
Принадлежит:

The invention relates to a method for continuous production of nitrobenzene by means of nitration of benzene with nitric acid and sulfuric acid, in which load change (i.e. a reduction or increase in the quantity of nitric acid supplied to the process per time interval) is particularly advantageously developed. The invention particularly relates to a method in which, in the case of a load reduction, the ratio of the masses of benzene and nitric acid supplied per time interval is significantly increased compared to said ratio before the load change and/or the ratio of the masses of nitric acid and sulfuric acid supplied per time interval is significantly reduced compared to said ratio before the load change. In the event of a load increase, the reverse is carried out. 1. A continuously operated process for preparing nitrobenzene , comprising nitrating benzene with nitric acid and sulfuric acid , wherein [{'sub': 1', '10, 'a stream containing benzene and having a proportion by mass of benzene wwith a mass flow rate of {dot over (m)},'}, {'sub': 2', '20, 'a stream containing nitric acid and having a proportion by mass of nitric acid wwith a mass flow rate of {dot over (m)}, and'}, {'sub': 3', '30, 'a stream containing sulfuric acid and having a proportion by mass of sulfuric acid wwith a mass flow rate of {dot over (m)};'}], '(i) the nitration is supplied with'}{'sub': 10', '20', '1', '2, '(ii) {dot over (m)}and {dot over (m)}, for given values of wand w, are chosen such that benzene is in a stoichiometric excess relative to nitric acid; and'}{'sub': '20', 'claim-text': [{'sub': 2', '20', '2', '1', '10', '1', '3', '30', '3, 'from a starting state A defined by a mass flow rate of nitric acid {dot over (m)}(A)={dot over (m)}(A)·w(A), a mass flow rate of benzene {dot over (m)}(A)={dot over (m)}(A)·w(A) selected with regard to (ii) and a mass flow rate of sulfuric acid {dot over (m)}(A)={dot over (m)}(A)·w(A),'}, {'sub': 2', '20', '2', '1', '10', '1', '3', '30', '3, 'to a ...

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Номер записи: 43
28-01-2016 дата публикации

Metallorganocatalysis For Asymmetric Transformations

Номер: US20160023198A1
Автор: Xumu Zhang
Принадлежит: Rutgars State University Of New Jersey

A ligand having the structure or its enantiomer; (I) wherein: each one of R a , R b , R c and R d is selected from alkyl, cycloalkyl, and aryl; the bridge group is selected from CH 2 NH; *CH(CH 3 )NH(C*,R); and the organocatalyst is an organic molecule catalyst covalently bound to the bridge group. Also, a catalyst having the structure or its enantiomer: (II) wherein: each one of R a , R b , R c and R d is selected from alkyl, cycloalkyl, and aryl; the bridge group is selected from CH 2 NH; *CH(CH 3 )NH(C*,R); and *CH(CH 3 )NH(C*,S); the organocatalyst is an organic molecule catalyst covalently bound to the bridge group; and M is selected from the group consisting of Rh, Pd, Cu, Ru, Ir, Ag, Au, Zn, Ni, Co, and Fe.

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Номер записи: 44
25-01-2018 дата публикации

PROCESS AND INTERMEDIATES FOR THE PREPARATION OF NEP INHIBITORS

Номер: US20180022690A1
Автор: MANDRELLI Francesca, MARTIN Benjamin, VENTURONI Francesco
Принадлежит:

The present invention relates to a new chemical synthesis, intermediates and catalysts useful for the preparation of the neprilysin (NEP) inhibitor sacubitril. It further relates to new intermediate compounds and their use for said new chemical synthesis route. 7. The process according to claim 6 , comprising the step of simultaneously or separately esterifiying the obtained compound of formula (1) claim 6 , or a salt thereof claim 6 , wherein R1 is hydrogen claim 6 , with a C-C-aliphatic alcohol claim 6 , to yield the compound of formula (1) wherein R1 is C-C-alkyl.15. (canceled)19. (canceled)21. (canceled)24. (canceled) The present invention relates to a new chemical synthesis route and intermediates useful for the preparation of neprilysin (NEP) inhibitors and their prodrugs, in particular for the NEP inhibitor prodrug sacubitril.The NEP inhibitor prodrug sacubitril (N-(3-carboxyl-1-oxopropyl)-(4S)-(p-phenylphenylmethyl)-4-amino-(2R)-methyl butanoic acid ethyl ester; IUPAC name 4-{[(1S,3R)-1-([1,1′-biphenyl]-4-ylmethyl)-4-ethoxy-3-methyl-4-oxobutyl]amino}-4-oxobutanoic acid) is represented by the following formula (A)Sacubitril together with valsartan, a known angiotensin receptor blocker (ARB), forms a sodium salt hydrate complex, known as LCZ696, comprising the anionic forms of sacubitril and valsartan, sodium cations and water molecules in the molar ratio of 1:1:3:2.5, respectively (ratio of 6:6:18:15 in the asymmetric unit cell of the solid state crystal), and which is schematically present in formula (B).Said complex is also referred to by the following chemical names: Trisodium [3-((1S,3R)-1-biphenyl-4-ylmethyl-3-ethoxycarbonyl-1-butylcarbamoyl)propionate-(S)-3′-methyl-2′-(pentanoyl{2″-(tetrazol-5-ylate)biphenyl-4′-ylmethyl}amino)butyrate] hemipentahydrate or Octadecasodium hexakis(4-{[(1S,3R)-1-([1,1′-biphenyl]-4-ylmethyl)-4-ethoxy-3-methyl-4-oxobutyl]amino}-4-oxobutanoate) hexakis(N-pentanoyl-N-{[2′-(1H-tetrazol-1-id-5-yl)[1,1′-biphenyl]-4-yl]methyl}-L- ...

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Номер записи: 45
24-01-2019 дата публикации

METHOD FOR SYNTHESIZING IODO- OR ASTATOARENES USING DIARYLIODONIUM SALTS

Номер: US20190023646A1
Автор: BRECHBIEL Martin W., Gestin Jean-Francois, Guerard Francois, LEE Yong-Sok
Принадлежит:

The present invention concerns a method of synthesizing a iodo- or astatoarene comprising the reaction of a diaryliodonium compound with a iodide or astatide salt, respectively. The invention also relates to said iodo- or astatoarene and diaryliodonium compound as such. The invention also concerns a method of synthesizing a iodo- or astatolabelled biomolecule and/or vector using said iodo- or astatoarene. 4. The method according to claim 1 , wherein the iodo- or astatoarene is of formula (I):{'br': None, 'Ar—X \u2003\u2003(I)'}wherein:X is I or At; and{'sub': 1', '2, 'Ar is Aror Ar.'}5. The method according to claim 1 , wherein the iodine or astatide salt is of formula (III):{'br': None, 'sup': +', '−, 'AX\u2003\u2003(III)'}wherein:{'claim-ref': {'@idref': 'CLM-00004', 'claim 4'}, 'X is as defined in ; and'}A is a monovalent cation selected among Na, K, Cs, tetraalkylammonium and tetraalkylphosphonium.6. The method according to claim 1 , wherein X is radioactive.7. The method according to claim 6 , wherein X is At.8. The method according to claim 6 , wherein X is I.9. The method according to claim 1 , wherein the reaction is carried out in a solvent selected from the group consisting of: acetonitrile claim 1 , an alcohol such as methanol claim 1 , dimethylformamide claim 1 , water claim 1 , and mixtures thereof.10. The method according to claim 1 , further comprising an astatide or iodide salt, and the diaryliodonium salt of formula (II) are insoluble, and', 'said iodo- or astatoarene is soluble., 'a purification step wherein a iodo- or astatoarene is extracted by a solvent in which11. The method of synthesizing an astatoarene according to claim 1 , previously comprising a step of reduction of astatine.12. A method of synthesizing a iodo- or astatolabeled biomolecule and/or vector comprising the steps of:{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, '(i) synthesizing a iodo- or astatoarene according to the method of ;'}(ii) reacting said iodo- or astatoarene ...

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Номер записи: 46
02-02-2017 дата публикации

HALOGENATED ANILINE AND METHOD FOR PRODUCING SAME

Номер: US20170029361A1
Автор: Inoue Hiroki, ITO Yoshikazu, KITAYAMA Takashi, Kobayashi Shinichi, Sakata Yuzuru
Принадлежит: NIPPON SODA CO., LTD.

The present invention provides a halogenated aniline represented by formula (I) (wherein each of Xand Xindependently represents a chlorine atom, a bromine atom or an iodine atom), a method for producing the halogenated aniline, and other aspects. 1. (canceled)34.-. (canceled)6. The method for producing a halogenated nitrobenzene according to claim 5 , wherein fuming sulfuric acid and concentrated nitric acid are added to the halogenated benzene represented by formula (III) to nitrate the halogenated benzene.7. The method for producing a halogenated nitrobenzene according to claim 5 , wherein fuming sulfuric acid and fuming nitric acid are added to the halogenated benzene represented by formula (III) to nitrate the halogenated benzene.810.-. (canceled)11. A method for producing 1 claim 5 ,2-dichloro-4 claim 5 ,5-difluorobenzene claim 5 , comprising a step of chlorinating 1 claim 5 ,2-difluorobenzene. The present invention relates to a novel halogenated aniline, which can be used as a production raw material for compounds that are useful as electronic materials, medicines, and agricultural chemicals and the like, as well as a method for producing the halogenated aniline.Priority is claimed on Japanese Patent Application No. 2012-280691, filed Dec. 25, 2012, the content of which is incorporated herein by reference.The compound 2,3-difluoroaniline is the starting raw material for producing 2-[2-fluoro-6-(7,8-difluoro-2-methylquinolin-3-yloxy)phenyl]propan-2-ol and 2-[2-fluoro-6-(7,8-difluoroquinolin-3-yloxy)phenyl]propan-2-ol, which are known as active ingredients for agricultural and horticultural germicides (Patent Document 1).Further, 2,3-difluoroaniline is also used in the production of medicines such as antibiotics (Patent Document 2), c-Met protein kinase inhibitors (Patent Document 3), drugs for Alzheimer's disease (Patent Document 4), Aurora B kinase inhibitors (Patent Document 5), and drugs for neuropathic pain (Patent Document 6).Moreover, 2,3-difluoroaniline ...

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Номер записи: 47
29-01-2015 дата публикации

Modulators of atp-binding cassette transporters

Номер: US20150031722A1
Автор: Anna Hazlewood, Ashvani Singh, Fredrick Van Goor, Jason Mccartney, Jinglan Zhou, Peter Grootenhuis, Sara Hadida-Ruah
Принадлежит: Vertex Pharmaceuticals Inc

The present invention relates to modulators of ATP-Binding Cassette (“ABC”) transporters or fragments thereof, including Cystic Fibrosis Transmembrane Conductance Regulator, compositions thereof, and methods therewith. The present invention also relates to methods of treating ABC transporter mediated diseases using such modulators.

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Номер записи: 48
29-01-2015 дата публикации

SAFE METHOD FOR PRODUCING ALKYL NITRATE

Номер: US20150031909A1
Автор: Mao Hengtao, Xu Deliang
Принадлежит:

The present invention provides a method for producing alkyl nitrate. The centrifugal extraction equipment acts as the esterification separator; a mixed acid solution containing sulfuric acid and nitric acid enters from the heavy phase inlet of the centrifugal extraction equipment; alkyl alcohol enters from the light phase inlet of the centrifugal extraction equipment; the feeding molar ratio of alkyl alcohol and nitric acid equals to 1:1.0-3.0; esterification reaction occurs with the mixed acid and alkyl alcohol at a temperature of 10˜60° C. under the rotating speed of 800-2000 r/min; under the action of centrifugal force, the generated coarse ester as a light phase and the spent acid as a heavy phase are separated; coarse ester as a light phase is discharged through the light-phase outlet of the centrifugal extractor; the spent acid as a heavy phase is discharged through the heavy-phase outlet of the centrifugal extractor; after alkali washing and water washing conventionally, coarse ester is dehydrated for drying and purified, then the refining products of alkyl nitrate is obtained. In the method of the present invention, esterification reaction, the separation of reaction products and the spent acid are finished in the same reactor simultaneously, which reduces the contact time of reaction products with the spent acid greatly, avoids the side reaction effectively, and ensures the safety of esterification process. 1. A method for producing alkyl nitrate , wherein , comprising the steps of:1) The centrifugal extraction equipment acts as the esterification separator; a mixed acid solution containing sulfuric acid and nitric acid enters from the heavy phase inlet of the centrifugal extraction equipment; alkyl alcohol enters from the light phase inlet of the centrifugal extraction equipment; the feeding molar ratio of alkyl alcohol and nitric acid equals to 1:1.0-3.0; esterification reaction occurs with the mixed acid and alkyl alcohol at a temperature of 10˜60° C. ...

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Номер записи: 49
31-01-2019 дата публикации

PHOSPHINE SUBSTITUTED FERROCENYL COMPLEX

Номер: US20190031697A1
Автор: AZIZ Md. Abdul, HELAL Aasif, SHAIKH M. Nasiruzzaman
Принадлежит: KING FAHD UNIVERSITY OF PETROLEUM AND MINERALS

A functionalized magnetic nanoparticle including an organometallic sandwich compound and a magnetic metal oxide. The functionalized magnetic nanoparticle may be reacted with a metal precursor to fol in a catalyst for various C—C bond forming reactions. The catalyst may be recovered with ease by attracting the catalyst with a magnet. 2. (canceled)3. The complex of claim 1 , wherein Ris an optionally substituted alkyl.4. The complex of claim 1 , wherein Ris an optionally substituted aryl.5. The complex of claim 1 , wherein X is NH.620-. (canceled) This application claims the priority of the filing date of the U.S. Provisional Patent Application No. 62/406,449 filed Oct. 11, 2016, the disclosure of which is hereby incorporated herein by reference in its entirety.This project was funded by the National Plan for Science, Technology and Innovation (MAARIFAH)-King Abdulaziz City for Science and Technology through the Science and Technology Unit at King Fahd University of Petroleum and Minerals (KFUPM), the Kingdom of Saudi Arabia, award number 15-NAN4650-04.Aspects of this technology are described in an article “Magnetic nanoparticle-supported ferrocenylphosphine: a reusable catalyst for hydroformylation of alkene and Mizoroki-Heck olefination” by M. Nasiruzzaman Shaikh, Md. Abdul Aziz, Aasif Helal, Mohamed Bououdina, Zain H. Yamania, and Tae-Jeong Kim, in RSC Advances, 2016, pages 41687-41695, which is incorporated herein by reference in its entirety.The present disclosure relates to a functionalized magnetic nanoparticle including an organometallic sandwich compound and a functional group which can bind to a nanoparticle. The disclosure also relates to a magnetic catalyst which catalyzes C—C bond forming reactions such as hydroformylation and the Mizoroki-Heck coupling reaction.Carbon-carbon bond formation reactions mediated by various transition metals have emerged as increasingly important methodologies for the preparation of numerous organic building blocks for drugs, ...

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Номер записи: 50
04-02-2021 дата публикации

RADIOLABELING AGENTS, METHODS OF MAKING, AND METHODS OF USE THEREOF

Номер: US20210032184A1
Автор: HASKALI Mohammad Baqir, PIKE Victor William, TELU Sanjay, YANG Bo Yeun
Принадлежит:

Described herein are labeling agents, specifically [C]fluoroform, [C]difluoromethane, [C]fluoromethyl iodide, [C]fluoromethyl bromide, [C]fluoromethyl chloride, [C]fluoromethyl trifluoromethansulfonate, [C]difluoromethyl iodide, [C]difluoromethyl bromide, [C]difluoromethyl chloride, [C]difluoromethyl trifluoromethansulfonate, [C]trifluoromethyl iodide, [C]trifluoromethyl bromide, [C]trifluoromethyl chloride, [C]trifluoromethyl trifluoromethansulfonate, []fluoroform, [F]difluoromethane, [F]difluoromethyl bromide or [F]trifluoromethyl bromide. Also included are methods of labeling precursors to provide labeled fluoroalkanes and imaging methods. 1. A gas phase solvent-free method for producing an C- or F-labeled fluoroalkane , the method comprising{'sup': 11', '18', '18', '11', '11, 'sub': 11', '11', '3, 'contacting [C]methane, [F]fluoromethane, [F]fluoromethyl bromide, [C]methyl iodide, [C]methyl bromide, [C]methyl chloride, or [C]methyl trffluoromethansuifonate, with CoFat a temperature of 50 to 450° C., and'}{'sup': 11', '18, 'isolating the C- or F-labeled fluoroalkane that is produced.'}2. The method of claim 1 , wherein{'sup': 11', '11, 'the precursor is [C]methane and the labeled fluoroalkane is [C]fluoroform,'}{'sup': 18', '18, 'the precursor is [F]fluoromethane and the labeled fluoroalkane is [F]fluoroform,'}{'sup': 18', '18, 'the precursor is [F]fluoromethane and the labeled fluoroalkane is [F]difluoromethane,'}{'sup': 18', '18, 'the precursor is [F]fluoromethyl bromide and the labeled fluoroalkane is [F]difluoromethyl bromide,'}{'sup': 18', '18, 'the precursor is [F]fluoromethyl bromide and the labeled fluoroalkane is [F]trifluoromethyl bromide,'}{'sup': 11', '11, 'the precursor is [C]methyl iodide and the labeled fluoroalkane is [C]fluoromethyl iodide,'}{'sup': 11', '11, 'the precursor is [C]methyl bromide and the labeled fluoroalkane is [C]fluoromethyl bromide,'}{'sup': 11', '11, 'the precursor is [C]methyl chloride and the labeled fluoroalkane is [C] ...

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Номер записи: 51
05-02-2015 дата публикации

Process for the Preparation of Nitroalcohols

Номер: US20150038746A1
Автор: Green G. David, Moore David W.
Принадлежит:

A process of preparing a nitroalcohol, e.g., 2-nitro-2-methyl-1-propane, from a nitropolyol, e.g., 2-nitro-2 -methyl-1,3-propanediol, the process comprising the step of contacting under hydrogenation conditions the nitropolyol with hydrogen, a hydrogenation catalyst and, optionally, a chelating agent. 1. A process of preparing a nitroalcohol from a nitropolyol , the process comprising the step of contacting at a temperature of 25-120° C. and a pressure of 300-1400 psi a nitropolyol with hydrogen and a hydrogenation catalyst , wherein the hydrogenation catalyst is at least one of a platinum group metal or a precious metal.2. (canceled)3. (canceled)4. The process of in which the hydrogenation catalyst is used in combination with a chelating agent.5. The process of in which the chelating agent is at least one of diethylenetriaminiepentaacetic acid (DTPA) claim 4 , ethylenediaminetetraacetic acid (EDTA) claim 4 , N claim 4 ,N′-bis(2-hydroxyethyl)ethylenediamine-N claim 4 ,N′-diacetic acid (HEEDA) claim 4 , N-2-hydroxyethyl-iminodiacetic acid (HEIDA) and nitrilotriacetic acid (NTA).6. The process of in which the amount of chelating agent used on a weight to weight basis with the catalyst metal is 1:1 to 1.5:1.7. The process of in which the nitropolyol is at least one of 2-nitro-2-methyl-1 claim 6 ,3-propanediol and tris(hydroxymethyl)nitromethane.8. A process of preparing a nitroalcohol from a nitroalkane claim 6 , the process comprising the steps of:A. Contacting under alkaline conditions a nitroalkane, an alcohol aldehyde and an alkaline catalyst to form a nitropolyol, andB. Contacting at a temperature of 25-120° C. and a pressure of 300-1400 psi the nitropolyol of A with hydrogen, a hydrogenation catalyst and, optionally, a chelating agent, wherein the hydrogenation catalyst is at least one of a platinum group metal or a precious metal. 1. Field of the InventionThis invention relates to a process of producing nitroalcohols by the reductive dehydroxylation of ...

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Номер записи: 52
11-02-2016 дата публикации

Utilizing Nitrate Salts in Order to Produce Explosives

Номер: US20160039722A1
Автор: Iman Sheikh
Принадлежит: Individual

Mass production of industrial explosives with one-tenth of the cost of the current production method—Nitric acid 98% removal of the chemical reaction producing explosive materials—Increasing the production safety—Producing ammonium sulfate, a chemical fertilizer, as a byproduct—Supporting the production of different explosives such as TNT, nitroglycerine and etc.—decreasing the acid concentration in the product.

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Номер записи: 53
11-02-2016 дата публикации

Activation of carbonyl beta-carbons for chemical transformations

Номер: US20160039827A1
Автор: Yonggui CHI, Zhenqian Fu
Принадлежит: NANYANG TECHNOLOGICAL UNIVERSITY

The present invention relates to a method for synthesizing a compound of Formula (I) as defined herein, comprising: (i) activating a compound of Formula (II) as defined herein, by reacting said compound of Formula (II) with a compound of Formula (III) as defined herein, in the presence of a base, to obtain a compound of Formula (IV) as defined herein; and (ii) reacting the compound of Formula (IV) with an electrophile to obtain the compound of Formula (I). The present invention further relates to the organocatalysts used in the described methods and their respective uses.

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Номер записи: 54
09-02-2017 дата публикации

PHENYL BENZYL ETHER DERIVATIVE AND PREPARATION METHOD AND APPLICATION THEREOF

Номер: US20170037008A1
Автор: Cui Mengchao, GUO Yuzhi, Lin Chunping, Liu Boli, Zhang Zhiyong
Принадлежит:

Parts of compounds, after being labeled by radionuclide, of the phenyl benzyl ether derivative, are used as Aβ plaque imaging agent. The structural formula of the phenyl benzyl ether derivative is shown by formula (I). The present invention develops a kind of brand new phenyl benzyl ether derivative which has high affinity with Aβ plaques in brains of AD patients. The chemical structure of the phenyl benzyl ether derivative is different from that of compounds disclosed in the prior art and the phenyl benzyl ether derivative belongs to a brand new compound for diagnosing and treating AD. The obtained Aβ plaque imaging agent has the advantages that the in-vivo stability is good, the fat solubility is low, the removal speed for the brain is fast, the problem of removing the radionuclide in vivo does not exist, and the application prospect and the market value are great. 115-. (canceled)17. The phenyl benzyl ether derivative according to claim 16 , wherein Rand Rare o-substituents claim 16 , m-substituents or p-substituents.18. The phenyl benzyl ether derivative according to claim 16 , wherein the halogen is fluorine claim 16 , chlorine claim 16 , bromine or iodine; the alkoxy is C-Calkoxy claim 16 , preferably C-Calkoxy; the alkyl is C-Calkyl claim 16 , preferably C-Calkyl; the carbocyclic alkyl is three-membered to six-membered carbocyclic alkyl claim 16 , preferably cyclopropyl claim 16 , cyclopentyl or cyclohexyl; heterocyclic alkyl is three-membered to six-membered heterocyclic alkyl claim 16 , preferably piperidyl claim 16 , piperazinyl or morpholine cyclic group; the alkylamino is C-Calkylamino claim 16 , preferably C-Calkylamino claim 16 , more preferably N-methylamino claim 16 , dimethylamino claim 16 , diethylamino claim 16 , dipropylamino or diisopropylamino; the aryl is phenyl or naphthyl; the heteraryl is pyridyl claim 16 , furyl claim 16 , thienyl claim 16 , benzothiazolyl claim 16 , benzofuryl or benzoxazolyl; the arylalkoxy is C-Caryl C-Calkoxy claim 16 ...

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Номер записи: 55
18-02-2016 дата публикации

SYNTHESIS OF (2-NITRO)ALKYL (METH)ACRYLATES VIA TRANSESTERIFICATION OF (METH)ACRYLATE ESTERS

Номер: US20160046558A1
Автор: Sathiosatham Muhunthan, Wilczynski Robert
Принадлежит:

Provided is a process for making (2-nitro)alkyl (meth)acrylate compounds of formula I: wherein n, R, R, R, R, R, R, R, and n are as defined herein, by a transesterification reaction between a nitroalcohol compound and a (meth)acrylate compound in the presence of a transesterification catalyst and a free radical inhibitor. 2. The process of wherein the transesterification catalyst is dibutyltin oxide claim 1 , a zirconium complex claim 1 , a hafnium complex claim 1 , a tetra-alkoxy titanate claim 1 , lithium hydroxide claim 1 , barium oxide claim 1 , magnesium oxide claim 1 , strontium oxide claim 1 , calcium oxide claim 1 , magnesium methylate claim 1 , 1 claim 1 ,4-diazabicyclo[2.2.2]octane claim 1 , a basic ion exchange resin claim 1 , or a mixture of two or more thereof.3. The process of wherein the transesterification catalyst is dibutyltin oxide claim 1 , a zirconium complex claim 1 , a hafnium complex claim 1 , 1 claim 1 ,4-diazabicyclo[2.2.2]octane claim 1 , or a mixture of two or more thereof.4. The process of wherein the transesterification catalyst is a zirconium complex.5. The process of wherein the mole ratio of (meth)acrylate compound to nitroalcohol is from 1:1 to 20:1.6. The process of wherein excess (meth)acrylate and its corresponding alcohol form an azeotropic mixture and wherein this byproduct alcohol is removed by azeotropic distillation.7. The process of wherein the free-radical inhibitor is claim 1 , phenothiazine claim 1 , hydroquinone claim 1 , methyl ether of hydroquinone claim 1 , 4-Hydroxy-TEMPO claim 1 , or mixtures thereof.8. The process of wherein Ris H and Ris H or linear or branched C-Calkyl optionally substituted with NO.9. The process of wherein Rand R′ are independently linear or branched C-Calkyl claim 1 , or Rand R′ claim 1 , together with the carbon atom to which they are attached claim 1 , form C-Ccycloalkyl.10. The process of wherein the compound of formula I is: 2-methyl-2-nitropropyl acrylate; 2-methyl-2-nitropropyl ...

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Номер записи: 56
01-05-2014 дата публикации

GEM-DINITRO ESTER COMPOUND AS ENERGETIC MATERIAL AND PREPARATION METHOD THEREOF

Номер: US20140121401A1
Автор: KIM Jin-Seuk, Kim Seung-Hee
Принадлежит: AGENCY FOR DEFENSE DEVELOPMENT

Provided is a gem-dinitro ester compound, represented by Formula 1 below: 2. The gem-dinitro ester compound of claim 1 , wherein the substituted or unsubstituted straight-chain or side-chain alkyl group of C˜Cis a substituted or unsubstituted straight-chain or side-chain butyl group claim 1 , pentyl group claim 1 , hexyl group claim 1 , heptyl group or octyl group.4. The method of claim 3 , wherein the substituted or unsubstituted straight-chain or side-chain alkyl group of C˜Cis a substituted or unsubstituted straight-chain or side-chain butyl group claim 3 , pentyl group claim 3 , hexyl group claim 3 , heptyl group or octyl group.5. The method of claim 3 , wherein the reaction of the compound represented by Formula 2 with the compound represented by Formula 3 is performed in the presence of a strong base.6. The method of claim 3 , wherein the reaction of the compound represented by Formula 2 with the compound represented by Formula 3 is performed using at least one solvent selected from the group consisting of lower alcohols of C˜Cand water. This application claims the benefit of Korean Patent Application No. 10-2012-0121335, filed on Oct. 30, 2012, which is hereby incorporated by reference in its entirety into this application.1. Technical FieldThe present invention relates to gem-dinitro ester compounds as energetic materials and a method of preparing the same.2. Description of the Related ArtA composite explosive has been developed in order to improve both performance and insensitivity of an explosive. Generally, a composite explosive includes a granular molecular explosive, such as a research development explosive (RDX), to provide explosiveness, and a binder composition. The binder composition is used in an amount of 2˜20 wt % based on the total amount of the composite explosive, and functions to provide dimensional stability and obtuseness to the granular molecular explosive. However, the binder composition does not have a nitro group for exhibiting ...

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Номер записи: 57
25-02-2016 дата публикации

METAL-CATALYZED COUPLING OF ARYL AND VINYL HALIDES WITH ALPHA, ALPHA-DIFLUOROCARBONYL COMPOUNDS

Номер: US20160052854A1
Автор: CHAKADAJ Wojciech, GE Shaozhong, Hartwig John F.
Принадлежит:

The coupling of aryl, heteroaryl, and vinyl halides with α,α-difluoroketones or silyl ethers or siylenol ethers of α,α-difluoroketones and α,α-difluoroamides and esters are described. Further derivatization of the coupling products (such as ketone cleavage and Baeyer-Villiger oxidation) is also described. 2. The composition according to claim 1 , wherein said complex is present in said composition in an amount of less than 10 mol % relative to said α claim 1 ,α-difluoromethyl carbonyl compound.3. The composition according to claim 2 , wherein said complex is present in said composition in an amount of about 2 mol % to about 5 mol % relative to said α claim 2 ,α-difluoromethyl carbonyl compound.5. The composition according to claim 4 , wherein said complex is present in said composition in an amount of less than 10 mol % relative to said silyl enol ether.6. The composition according to claim 5 , wherein said complex is present in said composition in an amount of about 2 mol % to about 5 mol % relative to said silyl enol ether.76. The composition according to any one of - claims 4 , wherein said composition does not contain BuSnF.87. The composition according to any one of - claims 4 , wherein said composition does not contain an organotin reagent.98. The composition according to any one of - claims 4 , wherein R claims 4 , R claims 4 , and Rare independently selected from unsubstituted C claims 4 , C claims 4 , C claims 4 , C claims 4 , Cand Calkyl.10. The composition according to claim 9 , wherein one or more of R claim 9 , R claim 9 , and Rare methyl.11. The composition according to any preceding claim claim 9 , further comprising a solvent.12. The composition according to claim 11 , wherein said solvent is a non-polar claim 11 , organic solvent.13. The composition according to claim 12 , wherein said solvent is toluene.14. The composition according to any preceding claim claim 12 , wherein said base is a member selected from CsCOand KPO.17. The composition ...

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Номер записи: 58
25-02-2016 дата публикации

NOVEL CURING AGENTS AND DEGRADEABLE POLYMERS AND COMPOSITES BASED THEREON

Номер: US20160052871A1
Автор: Li Xin, Liang Bo, Qin Bing
Принадлежит:

The present invention provides, among others, compounds of Formula (I) or a salt thereof, methods for making these compounds, degradable polymers and reinforced composites made therefrom, and methods for degrading and/or recycling the degradable polymers and reinforced composites. 2. The compound of claim 1 , wherein both m and n are 0.3. The compound of claim 1 , wherein both m and n are 1.4. The compound of claim 1 , wherein each of A and B claim 1 , independently claim 1 , is alkylene claim 1 , alkenylene claim 1 , arylene claim 1 , alkylene-arylene claim 1 , alkenylene-arylene claim 1 , alkynylene-arylene claim 1 , heteroarylene claim 1 , alkylene-heteroarylene claim 1 , alkenylene-heteroarylene claim 1 , or alkynylene-heteroarylene.5. The compound of claim 1 , wherein each of A and B claim 1 , independently claim 1 , is alkylene or arylene.6. The compound of claim 5 , wherein both A and B are claim 5 , at the same time claim 5 , alkylene or arylene.7. The compound of claim 6 , wherein both A and B are claim 6 , at the same time claim 6 , methylene claim 6 , ethylene claim 6 , or phenylene.8. The compound of claim 1 , wherein each of Rand R claim 1 , independently claim 1 , is hydrogen claim 1 , alkyl claim 1 , cycloalkyl claim 1 , heterocyclic claim 1 , heterocycloalkyl claim 1 , alkenyl claim 1 , cycloalkenyl claim 1 , aryl claim 1 , heteroaryl claim 1 , alkyl-hetero-alkyl claim 1 , alkynyl claim 1 , alkylene claim 1 , alkylene-hetero-alkylene claim 1 , alkenylene claim 1 , alkylene-hetero-alkenylene claim 1 , alkynylene claim 1 , or alkylene-hetero-alkynylene; or Rand R claim 1 , together with the carbon atom to which they are attached claim 1 , form a 3- to 7-membered saturated or unsaturated ring.9. The compound of claim 8 , wherein each of Rand R claim 8 , independently claim 8 , is hydrogen or alkyl claim 8 , or Rand R claim 8 , together with the carbon atom to which they are attached claim 8 , form a 3- to 7-membered saturated ring.10. The compound of ...

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Номер записи: 59
25-02-2021 дата публикации

Process of Fluorinating Inorganic or Organic Compounds by Direct Fluorination

Номер: US20210053911A1
Автор: DU Hongjun, Wu Wenting, Zhou Changyue
Принадлежит: Fujian Yongjing Technology Co., Ltd

The invention relates to a use of a fluorination gas, and the elemental fluorine (F) is present in a high concentration, for example, in a concentration of elemental fluorine (F), especially of equal to much higher than 15 or even 20% by volume, and to a process for the manufacture of a fluorinated compound by direct fluorination employing a fluorination gas, wherein the elemental fluorine (F) is present in a high concentration. The process of the invention is directed to the manufacture of a fluorinated compound, for the exception of fluorinated benzene, by direct fluorination. Especially the invention is of interest in the preparation of fluorinated organic compounds, final products and as well intermediates, for usage in agro-, pharma-, electronics-, catalyst, solvent and other functional chemical applications. The fluorination process of the invention may be performed batch-wise or in a continuous manner. 1. A process for the manufacture of a fluorinated compound by direct fluorination , wherein the process comprises the steps of:a) provision of a liquid medium comprising or consisting of a starting compound having one or more hydrogen atoms that are capable of being substituted by means of a halogenation reaction;{'sub': '2', 'b) provision of a fluorination gas comprising or consisting of elemental fluorine (F), wherein the fluorine is present in the fluorination gas in a high concentration of at least substantially more than, in particular very much more than 15% by volume (vol.-%), preferably equal to or more than 20% by volume (vol.-%);'}{'sub': '2', 'c) provision of a reactor or reactor system, resistant to elemental fluorine (F) and hydrogen fluoride (HF);'}{'sub': '2', 'd) passing the fluorination gas of b), in a reactor or reactor system of c), through the liquid medium of a) comprising or consisting of the starting compound, and thereby reacting the starting compound with the elemental fluorine (F) to substitute in the starting compound at least one of ...

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Номер записи: 60
13-02-2020 дата публикации

METHOD AND APPARATUS FOR PRODUCING ALKYL NITRITE

Номер: US20200048184A1
Автор: HINO Akira, II Hirofumi, NEGORO Naoki, NISHIDA Yoshikatsu
Принадлежит: UBE INDUSTRIES, LTD.

A method for producing an alkyl nitrite by bringing an aqueous solution containing nitric acid and an alkanol into contact with a gas including nitrogen monoxide and thereby producing an alkyl nitrite, in which the reaction temperature is 60° C. to 100° C., is provided. 1. A method for producing an alkyl nitrite , the method comprising:bringing an aqueous solution containing nitric acid and an alkanol into contact with a gas including nitrogen monoxide and thereby producing an alkyl nitrite, wherein a reaction temperature is 60° C. to 100° C.2. The method for producing an alkyl nitrite according to claim 1 , wherein a concentration of the alkanol is 50% by weight to 80% by weight with respect to the total amount of the aqueous solution.3. The method for producing an alkyl nitrite according to claim 1 , wherein a concentration of the alkanol is 60% by weight or more with respect to the total amount of the aqueous solution.4. The method for producing an alkyl nitrite according to claim 1 , wherein a concentration of nitric acid in a reaction liquid obtainable by bringing the aqueous solution into contact with the gas is decreased to 1% by weight or less.5. The method for producing an alkyl nitrite according to claim 1 , wherein the alkanol includes methanol.6. The method for producing an alkyl nitrite according to claim 1 , wherein a concentration of nitric acid in the aqueous solution is 1% by weight to 20% by weight with respect to the total amount of the aqueous solution.7. The method for producing an alkyl nitrite according to claim 1 , the method comprising:a first reaction step of producing the alkyl nitrite at a reaction temperature of 60° C. to 80° C.; anda second reaction step of producing the alkyl nitrite at a reaction temperature of 80° C. to 100° C.8. The method for producing an alkyl nitrite according to claim 7 , wherein a superficial gas velocity in the first reaction step is 20 mm/second to 100 mm/second claim 7 , and a superficial gas velocity in the ...

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Номер записи: 61
26-02-2015 дата публикации

Selective androgen receptor modulators

Номер: US20150057452A1
Автор: James David Rozzell, Raymond Mccague
Принадлежит: CATYLIX Inc

Compounds having therapeutic potential as androgen receptor modulators, and methods of making such compounds, are provided. The compounds are structurally related to bicalutamide but bear at least one difluoromethyl or C 2 to C 5 perfluoroalkyl group instead of a trifluoromethyl group.

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Номер записи: 62
03-03-2016 дата публикации

PROCESS FOR WORKING UP WASTE WATER FROM NITROBENZENE PREPARATION

Номер: US20160060152A1
Автор: Knauf Thomas, Mairata Antoni, Sluyts Erik, Van Tricht Jan
Принадлежит:

The invention relates to a process for working up alkaline waste water which is formed during washing of crude nitrobenzene obtained by nitration of benzene, wherein 1. A process for working up alkaline waste water which is formed during washing of crude nitrobenzene obtained by nitration of benzene , comprising:(i) heating the alkaline waste water to a temperature of from 150° C. to 500° C. under an increased pressure with respect to atmospheric pressure with exclusion of oxygen, wherein the heated alkaline waste water is then cooled and expanded;(ii) further purifying the waste water obtained in (i) by stripping with a stripping gas and then cooling the stripping gas stream loaded with impurities is then cooled to a temperature of from 10° C. to 60° C.; and(iii) separating the liquid process product obtained in (ii) into an aqueous and an organic phase and further using the organic phase obtained thereby in an aniline production process.2. The process of claim 1 , comprising sending the organic phase obtained in step (iii) to the educt stream of an aniline production plant.3. The process of claim 1 , comprising sending the organic phase obtained in step (iii) to the product stream of an aniline production plant.4. The process of claim 1 , comprising heating of the alkaline waste water in step (i) under an absolute pressure of from 50 bar to 350 bar.5. The process of claim 1 , comprising the heating of the alkaline waste water in step (i)6. The process of claim 1 , comprising claim 1 , after the heating claim 1 , cooling the alkaline waste water to a temperature of from 60° C. to 100° C.7. The process of claim 1 , comprising partially recycling the aqueous phase obtained in step (iii) into the stripping of sp (ii) and sending the remaining part which is not recycled to a biological treatment plant without further purification steps.8. The process of claim 1 , in which the alkaline waste water used in step (i) originates from step c) or step d) of the following ...

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Номер записи: 63
20-02-2020 дата публикации

METHOD OF SYNTHESIZING DICLOFENAC SODIUM

Номер: US20200055811A1
Автор: CHEN Fener, CHENG Dang, HUANG Zedu, LIANG Guanfeng, MENG Ge, Peng Haihui, WANG Lingdong
Принадлежит:

The invention relates to the chemical synthesis of pharmaceutical API, and specifically to a method of synthesizing diclofenac sodium, which is a kind of nonsteroidal anti-inflammatory drug for relieving pain. The method includes: nitrating phenylacetate to prepare o-nitrophenylacetate (2); hydrogenating o-nitrophenylacetate (2) to prepare o-aminophenylacetate (3); amidating an amino group of o-aminophenylacetate (3) to obtain 2-(2-benzoylaminophenyl) acetate (4); 2-(2-benzoylaminophenyl) acetate (4) reacting with thionyl chloride to prepare a chloroimine intermediate, and then condensing the intermediate of chloroimine with 2,6-dichlorophenol using an inorganic base to prepare (E)-methyl-2-(2-((2,6-dichlorophenoxy)(phenyl)methyleneamino) phenyl ester (5); subjecting (E)-methyl-2-(2-((2,6-dichlorophenoxy)(phenyl)methyleneamino) phenyl ester (5) to Chapman rearrangement to afford methyl 2-(2-(N-(2,6-dichlorophenyl)benzoylamino)phenyl) ester (6); and hydrolyzing methyl 2-(2-(N-(2,6-dichlorophenyl)benzoylamino)phenyl) ester (6) to provide the target compound as of diclofenac sodium API. The overall yield is up to 67% based on methyl phenylacetate. 1. A method of synthesizing diclofenac sodium , comprising:step (1) ortho-nitrating phenylacetate in a solution of dichloromethane containing a nitration agent to obtain o-nitrophenylacetate;step (2) hydrogenating o-nitrophenylacetate in the presence of a palladium catalyst to obtain o-aminophenylacetate;step (3) amidating the amino group of o-aminophenylacetate to obtain 2-(2-benzoylaminophenyl) acetate;step (4) 2-(2-benzoylaminophenyl) acetate reacting with thionyl chloride to obtain a chloroimine intermediate, and then condensing the chloroimine intermediate with 2,6-dichlorophenol using an inorganic base to obtain (E)-methyl-2-(2-((2,6-dichloro phenoxy)(phenyl)methyleneamino)phenyl) ester;step (5) subjecting (E)-methyl-2-(2-((2,6-dichlorophenoxy)(phenyl) methylene amino) phenyl) ester to Chapman rearrangement to obtain ...

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Номер записи: 64
04-03-2021 дата публикации

Growth inhibitor for forming thin film, method for forming thin film and semiconductor substrate prepared therefrom

Номер: US20210062338A1
Автор: Changbong YEON, Hyeran Byun, Jaesun Jung, Seokjong Lee, Sojung Kim, Taeho Song
Принадлежит: Soulbrain Co Ltd

The present invention relates to a growth inhibitor for forming a thin film, a method for forming a thin film using the same, and a semiconductor substrate prepared therefrom, and more particularly, to a growth inhibitor for forming a thin film represented by Chemical Formula 1 below, a method for forming a thin film using the same, and a semiconductor substrate prepared therefrom. A n B m X o   [Chemical Formula 1] wherein A is carbon or silicon, B is hydrogen or a C1-C3 alkyl, X is a halogen, n is an integer from 1 to 15, o is an integer of 1 or more, and m is from 0 to 2n+1. According to present invention, it is possible to suppress side reactions to appropriately lower a thin film growth rate and remove process byproducts in the thin film, thereby preventing corrosion or deterioration and greatly improving step coverage and thickness uniformity of a thin film even when the thin film is formed on a substrate having a complicated structure.

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Номер записи: 65
02-03-2017 дата публикации

Monomer, polymer, compensation film, optical film, and display device

Номер: US20170059755A1
Автор: Changki Kim, DMITRY Androsov, Joungeun YOO, Kitae Park
Принадлежит: SAMSUNG ELECTRONICS CO LTD

A monomer represented by Chemical Formula 1-1 wherein in Chemical Formula 1-1, Z, L 1 , L 2 , R 1 to R 6 , n, m, p, and a to f are the same as defined in the detailed description.

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Номер записи: 66
05-03-2015 дата публикации

Modulators of atp-binding cassette transporters

Номер: US20150065487A1
Автор: Anna Hazlewood, Ashvani Singh, Fred Van Goor, Jason Mccartney, Jinglan Zhou, Peter Grootenhuis, Sara Hadida-Ruah
Принадлежит: Vertex Pharmaceuticals Inc

The present invention relates to modulators of ATP-Binding Cassette (“ABC”) transporters or fragments thereof, including Cystic Fibrosis Transmembrane Conductance Regulator, compositions thereof, and methods therewith. The present invention also relates to methods of treating ABC transporter mediated diseases using such modulators.

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Номер записи: 67
05-03-2015 дата публикации

METHOD FOR PRODUCING NITROUS ACID ESTER, AND METHOD FOR PRODUCING DIALKYL OXALATE AND DIALKYL CARBONATE

Номер: US20150065742A1
Автор: Fukui Yuya, HINO Akira, II Hirofumi, TANAKA SYUJI, UEDA Satoshi
Принадлежит:

A method for producing nitrous acid ester in which nitric oxide, oxygen, and an alcohol are reacted, thereby generating nitrous acid ester includes a step of generating nitrous acid ester by supplying a bottom liquid from a bottom part of the reaction column, and nitric oxide and/or carbon monoxide, a step of supplying nitrous acid ester to the reaction column; a step of supplying a reaction liquid containing water, nitric acid, and the alcohol to a nitric acid condensing column from the reactor; and a step of separating a low-boiling point component by distillation from the reaction liquid under control of a concentration of the alcohol in a condensed liquid being generated at a bottom part of the nitric acid condensing column to be less than 4.0% by weight so as to introduce the condensed liquid into the reactor from the nitric acid condensing column. 1. A method for producing nitrous acid ester in which an alcohol is supplied to an upper part of a reaction column for producing nitrous acid ester , is made to flow downward from the upper part to a lower part of the reaction column , nitric oxide and oxygen , or a gas mixture thereof is supplied to the lower part of the reaction column , and nitric oxide , oxygen , and the alcohol are reacted , thereby generating nitrous acid ester , the method comprising:a step of extracting a bottom liquid containing water, nitric acid, and an alcohol from the bottom part of the reaction column so as to supply the bottom liquid to a reactor, and supplying nitric oxide and/or carbon monoxide to the reactor;a step of generating nitrous acid ester by brining nitric oxide and/or carbon monoxide into contact with the bottom liquid in the reactor;a step of supplying nitrous acid ester obtained in the reactor to the reaction column;a step of supplying a reaction liquid containing water, nitric acid, and the alcohol to a nitric acid condensing column from a lower part of the reactor; anda step of separating a low-boiling point component ...

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Номер записи: 68
28-02-2019 дата публикации

3,5-DIMETHOXYSTILBENE ANALOGS AND USES THEREOF

Номер: US20190059368A1
Автор: RIMANDO AGNES M., WENG JIAN-QUAN
Принадлежит:

Analogs of stilbene, and in particular, 3,5-dimethoxystilbene, are disclosed. Also disclosed are various uses for the different compounds described. The uses of the disclosed 3,5-dimethoxystilbene analogs include treatment as a pesticide, nematicide, fungicide, bactericide, and antimicrobial agent. Many of the analogs are novel, and procedures for synthesis are also provided. 1. A composition comprising a stilbene analog , wherein the stilbene analog is one of (Z)-1 ,3-dimethoxy-2-methyl-5-styrylbenzene (compound 7a) , (E)-1 ,3-dimethoxy-5-(3-methoxystyryl)-2-methylbenzene (compound 6b) , (Z)-1 ,3-dimethoxy-5-(3-methoxystyryl)-2-methylbenzene (compound 7b) , (E)-1 ,3-dimethoxy-5-(4-methoxystyryl)-2-methylbenzene (compound 6c) , (Z)-1 ,3-dimethoxy-5-(4-methoxystyryl)-2-methylbenzene (compound 7c) , (E)-1 ,3-dimethoxy-5-(4-nitrostyryl)-2-methylbenzene (compound 6d) , (Z)-1 ,3-dimethoxy-5-(4-nitrostyryl)-2-methylbenzene (compound 7d) , (E)-1 ,3-dimethoxy-5-(4-fluorostyryl)-2-methylbenzene (compound 6e) , (Z)-1 ,3-dimethoxy-5-(4-fluorostyryl)-2-methylbenzene (compound 7e) , (E)-1 ,3-dimethoxy-5-(4-chlorostyryl)-2-methylbenzene (compound 6f) , (Z)-1 ,3-dimethoxy-5-(4-chlorostyryl)-2-methylbenzene (compound 7f) , (E)-1 ,3-dimethoxy-5-(4-bromostyryl)-2-methylbenzene (compound 6g) , (Z)-1 ,3-dimethoxy-5-(4-bromostyryl)-2-methylbenzene (compound 7g) , (E)-1 ,3-dimethoxy-5-(4-trifluoromethylstyryl)-2-methylbenzene (compound 6h) , (Z)-1 ,3-dimethoxy-5-(4-trifluoromethylstyryl)-2-methylbenzene (compound 7h) , (E)-1 ,3-dimethoxy-5-(3 ,4-dichlorostyryl)-2-methylbenzene (compound 6i) , (Z)-1 ,3-dimethoxy-5-(3 ,4-dichlorostyryl)-2-methylbenzene (compound 7i) , (E)-1 ,3-dimethoxy-5-(2 ,4-dimethoxystyryl)-2-methylbenzene (compound 6j) , (Z)-1 ,3-dimethoxy-5-(2 ,4-dimethoxystyryl)-2-methylbenzene (compound 7j) , (E)-1 ,3-dimethoxy-5-(3 ,4-dimethoxystyryl)-2-methylbenzene (compound 6k) , (Z)-1 ,3-dimethoxy-5-(3 ,4-dimethoxystyryl)-2-methylbenzene (compound 7k) , (E)-1 ,3-dimethoxy-5-(3 ...

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Номер записи: 69
17-03-2022 дата публикации

Process for preparation of 2-amino-5-hydroxy propiophenone

Номер: US20220081388A1
Автор: Jagadeeswara Rao Dadi, Raj Koti Katkuri, Sridhar Tummu, Uma Maheswer Rao Vasirredi, Venkata Ramana Kintali
Принадлежит: Laurus Labs Pvt Ltd

The present invention relates to a process for preparation of 2-Amino-5-hydroxy propiophenone, a key intermediate for the synthesis of camptothecin analogs including 7-Ethyl-10-hydroxycamptothecin (SN-38).

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Номер записи: 70
08-03-2018 дата публикации

METHODS FOR meta-ARYLATION OF AROMATIC ALCOHOLS

Номер: US20180065909A1
Автор: Ferreira Eric, Li Qiankun
Принадлежит:

Provided are methods for the meta-selective C—H arylations of arene alcohol-based substrates. The methods combine the transient norbornene strategy with a quinoline-based acetal scaffold to achieve the formation of biaryl compounds. These processes establish a foundation for catalytic polyfunctionalization of alcohol-based compounds. The method comprises attaching a heterocyclic hemiacetal scaffold to an aromatic alcohol or a substituted aromatic alcohol; reacting the aromatic or substituted aromatic alcohol having the heterocyclic hemiacetal scaffold attached with an alkyl or aryl iodide in a reaction mix comprising a palladium catalyst, a silver salt, and carboxymethyl norbornene to generate a meta-arylated arene conjugated to the heterocyclic hemiacetal scaffold; and then cleaving the heterocyclic hemiacetal scaffold from the meta-arylated arene alcohol. 1. A method of meta-arylating an arene alcohol , the method comprising the steps of:(a) attaching a heterocyclic hemiacetal scaffold to an aromatic alcohol or a substituted aromatic alcohol;(b) reacting the aromatic or substituted aromatic alcohol having the heterocyclic hemiacetal scaffold attached thereto with an alkyl or aryl iodide in a reaction mix comprising a palladium catalyst, a silver salt, and carboxymethyl norbornene to generate a meta-arylated arene conjugated to the heterocyclic hemiacetal scaffold; and(c) cleaving the heterocyclic hemiacetal scaffold from the meta-arylated arene alcohol.2. The method of claim 1 , wherein in step (b) the reaction mix further comprises a ligand.3. The method of claim 1 , wherein the heterocyclic hemiacetal scaffold is quinolinyl hemiacetal benzoate.5. The method of claim 3 , wherein the aryl iodide is an iodoalkylbenzoate.6. The method of claim 5 , wherein the iodoalkylbenzoate is iodomethylbenzoate.7. The method of claim 2 , wherein the ligand is selected from the group consisting of acetylglycine claim 2 , 3-acetylamino 2-hydroxypyridine claim 2 , 3-[3-trifluoro 1- ...

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Номер записи: 71
29-05-2014 дата публикации

Process for making tertiary aminoalcohol compounds

Номер: US20140145108A1
Автор: Christian Spieker, David W. Moore, John D. Gummere
Принадлежит: ANGUS CHEMIE GMBH

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

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Номер записи: 72
09-03-2017 дата публикации

CONTINUOUS SYNTHESIS OF ISOOCTYL NITRATE IN A FLOW REACTOR

Номер: US20170066710A1
Автор: MA Bing, Shen Wei, Wang Yanhua, Zhang Mo
Принадлежит:

A process for synthesizing isooctyl nitrate in a continuous flow reactor comprises flowing a H2SO4—HNO3 mixture within a flow reactor, flowing isooctyl alcohol into said flow reactor so as to mix the isooctyl alcohol with the H2SO4—HNO3 mixture and produce a reaction mixture stream flowing in said reactor, maintaining the reaction mixture stream flowing in said flow reactor at a reaction temperature within in the range −10° to 35° C. inclusive, and wherein the residence time of the reaction mixture stream in the flow reactor is greater than or equal to 5 seconds and less than or equal to 40 seconds, and wherein the H2SO4 of the H2SO4—HNO3 mixture is H2SO4 having a concentration of in the range of 85 to 95% inclusive, more desirably 88 to 92% inclusive, most desirably of 90%. 1. A process for synthesizing isooctyl nitrate in a continuous flow reactor with 99% or greater conversion and 99% or greater yield , the process comprising:flowing a H2SO4—HNO3 mixture within a flow reactor;flowing isooctyl alcohol into said flow reactor so as to mix the isooctyl alcohol with the H2SO4—HNO3 mixture and produce a reaction mixture stream flowing in said reactor;maintaining the reaction mixture stream flowing in said flow reactor at a reaction temperature within in the range −10° to 35° C. inclusive,wherein the residence time of the reaction mixture stream in the flow reactor is in the range of 5 to 40 seconds, inclusive, and wherein the H2SO4 of the H2SO4—HNO3 mixture is H2SO4 having a strength within the range of 85% to 95% inclusive.2. The process according to wherein the H2SO4 of the H2SO4—HNO3 mixture is H2SO4 having a strength within the range of 88% to 92% inclusive.3. The process according to wherein the H2SO4 of the H2SO4—HNO3 mixture is 90% H2SO4.4. The process according to wherein the step of flowing a H2SO4—HNO3 mixture within a flow reactor comprises flowing a H2SO4 stream into a first inlet of the flow reactor and flowing a HNO3 stream into a second inlet of the flow ...

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Номер записи: 73
12-03-2015 дата публикации

METHOD FOR CONTINUOUS PRODUCTION OF NITROBENZENE

Номер: US20150073180A1
Автор: Knauf Thomas, Merkel Michael
Принадлежит: Bayer Intellectual Property GmbH

The invention relates to a method for producing nitrobenzene, in which crude nitrobenzene is first produced by nitrating benzene and said crude nitrobenzene is then washed in succession in at least one acid wash, in at least one alkaline wash and in at least one neutral wash, at least one additional wash with an aqueous solution of a potassium salt being interposed between the last alkaline wash and the first neutral wash. 1. Method for producing nitrobenzene bya) nitration of benzene with nitric acid or mixtures of nitric acid and sulfuric acid and subsequent phase separation into an aqueous phase and an organic phase containing nitrobenzene,b) washing of the organic nitrobenzene-containing phase obtained in step a) in at least one wash and subsequent phase separation into an aqueous phase and an organic phase containing nitrobenzene, sodium hydroxide, sodium carbonate and sodium hydrogen carbonate,', 'and subsequent phase separation into an aqueous phase and an organic phase containing nitrobenzene,, 'c) washing of the organic nitrobenzene-containing phase obtained in step b) in at least one alkaline wash with an aqueous solution of a base selected from the group consisting of'}d) washing of the organic nitrobenzene-containing phase obtained in step c) in at least one wash with an aqueous solution of a potassium salt and subsequent phase separation into an aqueous phase and an organic phase containing nitrobenzene,e) washing of the organic nitrobenzene-containing phase obtained in step d) in at least one neutral wash with water and subsequent phase separation into an aqueous phase and an organic phase containing nitrobenzene,f) processing of the organic nitrobenzene-containing phase obtained in step e), wherein purified nitrobenzene is obtained.2. Method according to claim 1 , wherein in step c) an aqueous solution of sodium hydroxide is used.3. Method according to or claim 1 , wherein in step d) a molar ratio of potassium to sodium ions of 1:1 to 20:1 is ...

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Номер записи: 74
17-03-2016 дата публикации

PROCESS FOR WORKING UP WASTE WATER FROM NITROBENZENE PREPARATION

Номер: US20160075582A1
Автор: Knauf Thomas, Mairata Antoni, Sluyts Erik, Van Tricht Jan
Принадлежит:

The present invention provides a process for working up alkaline waste water which is formed during washing of crude nitrobenzene obtained by nitration of benzene, wherein 1. A process for working up alkaline waste water which is formed during washing of crude nitrobenzene obtained by nitration of benzene , comprising:(i) heating the alkaline waste water to a temperature of from 150° C. to 500° C. under an increased pressure with respect to atmospheric pressure with exclusion of oxygen;(ii) adding a base to the waste water obtained in (i); and(iii) further purifying the waste water obtained in (ii) by stripping with a stripping gas and then cooling the stripping gas stream loaded with impurities to a temperature of from 10° C. to 60° C.2. The process of claim 1 , comprising heating the alkaline waste water in step (i) under an absolute pressure of from 50 bar to 350 bar.3. The process of claim 1 , comprising heating the alkaline waste water in step (i) for a period of from 5 minutes to 120 minutes.4. The process of claim 3 , comprising claim 3 , after the heating claim 3 , cooling the alkaline waste water to a temperature of from 60° C. to 100° C.5. The process according to one of claim 1 , in which the base used in step (ii) is an aqueous solution of a base selected from the group consisting of lithium hydroxide claim 1 , sodium hydroxide claim 1 , potassium hydroxide and rubidium hydroxide.6. The process of claim 1 , comprising adding the base in step (ii) such that a pH of at least 12 is established.7. The process of claim 1 , in which the stripping in step (iii) is carried out under an absolute pressure of from 0.5 bar to 2 bar and at a temperature of from 80° C. to 120° C.8. The process of claim 1 , in which the stripping gas is steam.9. The process of claim 1 , comprising purging organic constituents out of the stream obtained in step (iii) after cooling of the stripping gas stream loaded with impurities to a temperature of 10° C. to 60° C. claim 1 , to obtain ...

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Номер записи: 75
15-03-2018 дата публикации

PROCESS TO PREPARE 3-METHYL-2-NITROBENZOIC ACID BY AIR OXIDATION

Номер: US20180072653A1
Автор: Dumas Donald J.
Принадлежит:

A method for preparing 3-methyl-2-nitrobenzoic acid is disclosed wherein 1,3-dimethyl-2-nitrobenzene is combined with an oxidation catalayst in the presence of an oxygen source and an initiator, provided that less than 99% of the 1,3-dimethyl-2-nitrobenzene is oxidized. 2. The method of wherein Ris C-Calkyl or C-Ccycloalkyl.3. The method of wherein Ris methyl claim 2 , isopropyl claim 2 , cyclopropyl or t-butyl.4. The method of wherein Ris methyl or t-butyl.5. The method of wherein Ris C-Calkyl.6. The method of wherein Ris methyl or ethyl.7. The method of wherein Ris ethyl.8. The method of wherein the cyclizing agent is PBr.9. The method of wherein the chlorinating agent is HCl and HO.11. The method of wherein Ris C-Calkyl or C-Ccycloalkyl.12. The method of wherein Ris methyl claim 11 , isopropyl claim 11 , cyclopropyl or t-butyl.13. The method of wherein Ris methyl or t-butyl.14. The method of wherein Ris methyl.15. The method of wherein Ris t-butyl. A need exists for additional methods to prepare 3-methyl-2-nitrobenzoic acid that are selective and cost-effiective. 3-Methyl-2-nitrobenzoic acid is useful as in intermediate in the preparation of agrochemicals such as Rynaxypyr® and Cyazypyr®.Oxidation of mono-alkyl ortho-nitroalkylaromatic compounds is exemplified in Jacobsen, U.S. Pat. No. 5,591,890. Selective oxidation of one alkyl group in ortho-nitroalkylaromatic compounds with two or more alkyl groups is not disclosed in this patent.Oxidation of 2-nitro-p-xylene is disclosed in Jacobson and Ely, 1996, 68, 87-96. Selective oxidation of one alkyl group in ortho-nitroalkylaromatic compounds with two or more alkyl groups is not disclosed in this publication.Oxidation of 2-nitro-m-xylene is disclosed in JP05132450 using HSOand stoichiometric CrO.This invention provides a method for preparing a compound of Formula 2comprising, contacting a compound of Formula 1with an oxidation catalyst in the presence of an oxygen source and an initiator provided that less than 99% ...

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Номер записи: 76
07-03-2019 дата публикации

PROCESS FOR THE PREPARATION OF IOPAMIDOL

Номер: US20190071392A1
Автор: BATTISTINI Elisa, BUONSANTI Federica, IMPERIO Daniela, Lattuada Luciano, NAPOLITANO Roberta
Принадлежит: BRACCO IMAGING S.P.A.

The present invention discloses a process for the preparation of Iopamidol of formula (II) and comprising the following steps: a) reacting the Compound (I) wherein X is OR2 or R3, and wherein R2 and R3 are a Ci-C6 linear or branched alkyl, C3-C6 cycloalkyl, C6 aryl, optionally substituted with a group selected from the group consisting of methyl, ethyl, n-propyl, i-propyl, n-butyl, sec-butyl, t-butyl and phenyl, with the acylating agent (S)-2-(acetyloxy)propanoyl chloride in a reaction medium to provide the acetyloxy derivative of Compound (I); b) hydrolyzing the intermediate from step a) with an aqueous solution at a pH comprised from 0 to 7, by adding water or a diluted alkaline solution such as sodium hydroxide or potassium hydroxide, freeing the hydroxyls from the boron-containing protective groups, obtaining the N—(S)-2-(acetyloxy)propanoyl derivative of Compound (II); c) alkaline N hydrolysis to restore the (S)-2-(hydroxy)propanoyl group and to obtain Iopamidol (II) and optional recovery of the boron derivative from the solution obtained in step b). The boron-containing protective group is versatile, efficient and recyclable. A one-pot synthesis, without intermediate isolation is provided, leading to a decreasing of recovered and recycled solvents and a significant increasing in the yield, representing a significant advantage in terms of cost-effectiveness of the entire process and environmental awareness. 122-. (canceled)23. A process for recovery of a boronic acid of formula R—B(OH) , wherein Ris selected from the group consisting of C-Clinear or branched alkyl , C-Ccycloalkyl , and Caryl , optionally substituted with a group selected from the group consisting of methyl , ethyl , n-propyl , i-propyl , n-butyl , sec-butyl , t-butyl , and phenyl , from an aqueous mixture optionally comprising a polar solvent , said process comprising the following steps:admixing the aqueous mixture with a water-immiscible organic solvent in a weight ratio between the boronic ...

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Номер записи: 77
07-03-2019 дата публикации

Octahydroanthracene Compound, Preparation Method and Application Thereof

Номер: US20190071393A1
Автор: BAO Xuefei, CHEN Guoliang, FANG Wuhong, GAO Jinheng, REN Fulong, YUAN Chunling, ZHANG Daiming, ZHENG Zhonghui, ZHOU Linbo, ZOU Libo
Принадлежит:

An octahydroanthracene compound having the structure shown in formula (I) and (II), preparation method and application thereof are disclosed. The octahydroanthracene compound has a good therapeutic effect on tumors and neurodegenerative diseases. The preparation of the octahydroanthracene compound is mainly carried out by using benzene as a starting material, and being subjected to Friedel-Crafts reaction, nitration, reduction, (sulfo-) amide formation, reduction, urea formation or amide formation, thus obtaining a target compound. 2. The octahydroanthracene compound and the pharmaceutically acceptable salts of the octahydroanthracene compound of claim 1 , whereinthe Linker is a substituted/unsubstituted phenyl group, pyridine, furan, pyrrole, thiazole or thiophene; wherein a substituent of the substituted phenyl group, pyridine, furan, pyrrole, thiazole or thiophene is a C1-C6 alkyl group or a C1-C6 alkoxy group.3. The octahydroanthracene compound and the pharmaceutically acceptable salts of the octahydroanthracene compound of claim 1 , wherein the nitrogen-free structural fragment is C1-C10 alkyl group.5. The octahydroanthracene compound and the pharmaceutically acceptable salts of the octahydroanthracene compound of claim 1 , wherein X is hydrogen claim 1 , methyl or ethyl.6. An octahydroanthracene compound and pharmaceutically acceptable salts of the octahydroanthracene compound claim 1 , selecting from:4-[(1,1,4,4,5,5,8,8-octamethyl-1,2,3,4,5,6,7,8-octahydro-9-anthryl) carbamoyl] methyl benzoate;4-[(1,1,4,4,5,5,8,8-octamethyl-1,2,3,4,5,6,7,8-octahydro-9-anthryl) carbamoyl] benzoic acid;N-hydroxy-4-[(1,1,4,4,5,5,8,8-octamethyl-1,2,3,4,5,6,7,8-octahydro-9-anthryl) carbamoyl] benzamide;N-(2-aminophenyl)-4-[(1,1,4,4,5,5,8,8-octamethyl-1,2,3,4 5,6,7,8-octahydro-9-anthryl) carbamoyl] benzamide;N[2-(N,N-diethylamino)]ethyl-4-[(1,1,4,4,5,5,8,8-octamethyl-1,2,3,4,5,6,7,8-octahydro-9-anthryl) carbamoyl] benzamide;N-(2-amino) ethyl -4[(1,1,4,4,5,5,8,8-octamethyl-1,2,3,4,5 ...

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Номер записи: 78
05-03-2020 дата публикации

METHODS FOR MAKING QUINOLINYLDIAMINES

Номер: US20200071344A1
Автор: Canich Jo Ann M., Goryunov Georgy P., Hagadorn John R., SAMSONOV Oleg V., Sharikov Mikhail I., Titone Michelle E., Uborsky Dmitry Dmitry, VOSKOBOYNIKOV Alexander Z.
Принадлежит:

The present disclosure provides methods for making quinolinyldiamine products from quinolinyl starting materials. In addition, the quinolinyldiamines can be used as ligands or ligand precursors for catalysts, e.g. for use in olefin polymerization. 2. The method of claim 1 , wherein introducing comprises:mixing the acid solution with the compound represented by Formula C or Formula K to form a first mixture;mixing the nitrite with the first mixture to form a second mixture; andmixing the phosphorous oxoacid with the second mixture to form a third mixture.3. The method of claim 1 , further comprising contacting the compound represented by Formula D or Formula L with an organic solvent.4. The method of claim 3 , wherein the organic solvent is an alcohol.5. The method of claim 1 , wherein the acid solution is a 2M to 6M solution of HCl.6. The method of claim 1 , wherein the nitrite is sodium nitrite claim 1 , potassium nitrite claim 1 , or mixtures thereof.7. The method of claim 1 , wherein the phosphorous oxoacid is hypophosphorous acid.8. The method of claim 1 , further comprising:{'sub': '4', 'introducing TiCland an aniline to the compound represented by Formula D or Formula L.'}9. The method of claim 8 , wherein introducing comprises:{'sub': '4', 'mixing the TiClwith the aniline to form a fourth mixture;'}heating the fourth mixture at a temperature of from about 30° C. to about 120° C.;mixing the compound represented by Formula D or Formula L to form a fifth mixture;heating the fifth mixture at a temperature of from about 30° C. to about 120° C.; andobtaining a dried product from the fifth mixture.10. The method of claim 9 , further comprising introducing the dried product to a reducing agent and an acid.11. The method of claim 10 , wherein:{'sub': 4', '3', '4, 'the reducing agent is selected from NaBH, NaBHCN, and LiAlH, and'}the acid is acetic acid.13. The method of claim 12 , further comprising contacting the compound represented by Formula E or Formula M with an ...

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Номер записи: 79
05-06-2014 дата публикации

Modulators of atp-binding cassette transporters

Номер: US20140155431A1
Автор: Anna Hazlewood, Ashvani Singh, Fredrick Van Goor, Jason Mccartney, Jinglan Zhou, Peter Grootenhuis, Sara Hadida-Ruah
Принадлежит: Vertex Pharmaceuticals Inc

The present invention relates to modulators of ATP-Binding Cassette (“ABC”) transporters or fragments thereof, including Cystic Fibrosis Transmembrane Conductance Regulator, compositions thereof, and methods therewith. The present invention also relates to methods of treating ABC transporter mediated diseases using such modulators.

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Номер записи: 80
05-06-2014 дата публикации

PROCESS FOR PREPARING ARYL- AND HETEROARYLACETIC ACID DERIVATIVES

Номер: US20140155632A1
Автор: Gooßen Lukas J., Himmler Thomas, Rudolphi Felix, Song Bingrui
Принадлежит:

The invention relates to a process for preparing aryl- and heteroarylacetic acids and derivatives thereof by reaction of aryl or heteroaryl halides with malonic diesters in the presence of a palladium catalyst, of one or more bases and optionally of a phase transfer catalyst. This process enables the preparation of a multitude of functionalized aryl- and heteroarylacetic acids and derivatives thereof, especially also the preparation of arylacetic acids with sterically demanding substituents. 4. The process for preparing a compound of formula (III) according to claim 1 , whereAr is 1-naphthyl, 2-naphthyl, phenyl, 4-N,N-dimethylaminophenyl, 4-methylthiophenyl, 4-methoxyphenyl, 4-ethoxyphenyl, 3-methoxyphenyl, 2-methoxyphenyl, 2-methylphenyl, 3-methylphenyl, 4-methylphenyl, 4-fluorophenyl, 3-fluorophenyl, 2-fluorophenyl, 2-ethylphenyl, 4-ethoxycarbonylphenyl, 3-thienyl.5. The process for preparing a compound of formula (III) according to claim 1 , whereAr is 2,6-dimethylphenyl, 2,4,6-trimethylphenyl, 4-cyanophenyl, 4-cyano-2-methylphenyl, 3-cyanophenyl, 4-ethoxycarbonylphenyl, 4-trifluoromethylphenyl, 4-acetylphenyl, 4-nitrophenyl, 4-benzoylphenyl.6. The process for preparing a compound of formula (III) according to claim 1 , where{'sup': 6', '7, 'Rand Rare each ethyl.'}7. The process for preparing a compound of formula (III) according to claim 1 , wherein the palladium catalyst used is bis(dibenzylideneacetone)palladium claim 1 , tris(dibenzylideneacetone)dipalladium or palladium acetate.8. The process for preparing a compound of formula (III) according to claim 1 , wherein the phosphine ligand used is tri-tert-butylphosphine claim 1 , tricyclohexylphosphine claim 1 , tris(1-adamantyl)phosphine claim 1 , n-butyldi(1-adamantyl)phosphine (cataCXium® A) claim 1 , benzyldi(1-adamantyl)phosphine (cataCXium® ABn) claim 1 , 2-(di-tert-butylphosphino)biphenyl (JohnPhos) or 2-(dicyclohexylphosphino)-2′-(N claim 1 ,N-dimethylamino.9. The process for preparing a compound of ...

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Номер записи: 81
18-03-2021 дата публикации

METHOD FOR PREPARATION OF 5-FLUORO-2-METHYL-3-NITROBENZOIC ACID AND ITS METHYL ESTER

Номер: US20210078933A1
Автор: AELLIG Christof, Bersier Michael, FILLIGER Sarah, HANSELMANN Paul, KULESZA Anna
Принадлежит:

The invention discloses a method for preparation of 5-fluoro-2-methyl-3-nitrobenzoic acid and its methyl ester by conversion of 5-fluoro-2-methylbenzoic acid with fuming nitric acid and oleum and subsequent conversion with methanol. 2. Method according to claim 1 , wherein{'sub': 2', '4, 'the concentrated sulfuric acid has a content of from 94 to 100 wt % of HSO;'}the wt % based on the weight of the concentrated sulfuric acid.3. Method according to claim 1 , wherein{'sub': '3', 'the oleum contains 50 to 70 wt % of SO.'}4. Method according to claim 1 , wherein{'sub': '3', 'the fuming nitric acid has a content of from 95 to 100 wt % of HNO.'}5. Method according to claim 1 , wherein MIX contains{'sub': 2', '4, 'concentrated sulphuric acid in an amount of 4 to 12 times of molar equivalents of HSOrelative to compound of formula (1),'}{'sub': 2', '4, 'oleum in an amount of 1 to 4 times of molar equivalents of HSOrelative to compound of formula (1),'}{'sub': '3', 'fuming nitric acid in an amount of 1 to 2 times of molar equivalents of HNOrelative to compound of formula (1).'}6. Method according to claim 1 , wherein the amounts of concentrated sulfuric acid claim 1 , oleum and fuming nitric acid in MIX add up to 95 to 100 wt % claim 1 , more preferably to 98 to 100 wt % claim 1 , the wt % being based on the total weight of MIX; even more preferably MIX consists of concentrated sulfuric acid claim 1 , oleum and fuming nitric acid.7. Method according to claim 1 , wherein the reaction temperature TEMPI of REAC1 is from −10 to 30° C.8. Method according to claim 1 , wherein the reaction time TIME1 of REAC1 is from 1 sec to 2 h.9. Method according to claim 1 , wherein REAC1 is done in a continuous way.11. Method according to claim 10 , wherein{'sub': 2', '4, 'REAC2 is done in the presence of an acid ACID2, ACID2 is HSO.'}12. Method according to claim 10 , whereinboth REAC1 and REAC2 are done in a continuous way and are done consecutively without isolation of compound of formula ( ...

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Номер записи: 82
14-03-2019 дата публикации

PROCESS FOR THE PREPARATION OF IOPAMIDOL

Номер: US20190077745A1
Автор: BATTISTINI Elisa, BUONSANTI Federica, IMPERIO Daniela, Lattuada Luciano, NAPOLITANO Roberta
Принадлежит: BRACCO IMAGING S.P.A.

The present invention discloses a process for the preparation of Iopamidol of formula (II) 2. The method according to claim 1 , wherein X is OR.3. The method according to claim 1 , wherein X is R.5. The method according to claim 4 , wherein the boronic acid is selected from the group consisting of: phenylboronic acid claim 4 , tolylboronic acid and butylboronic acid or the boroxine (III) is selected from the group consisting of tri-phenylboroxine and tri-methylboroxine.8. The method according to claim 1 , further comprising the purification and isolation of Iopamidol (II).9. The method according to claim 8 , wherein said purification is to pharmaceutical grade. The present invention relates to the field of organic chemistry, in particular to the synthesis of iodinated contrast agents, more in particular to the use of boron oxyacids and derivatives thereof as protecting groups. The present invention provides also compounds useful as intermediates in the above synthesis.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-hydroxy-1-oxopropyl)amino]-2,4,6-triiodo-1,3-benzendicarboxamide) (II), whose structural formula is indicated below, is one of the numerous tri-iodinated diagnostic agents, commercially available and widely used for this purpose:The widespread use of this compound in ...

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Номер записи: 83
24-03-2016 дата публикации

PROCESS FOR THE PREPARATION OF NITROBENZENE BY ADIABATIC NITRATION

Номер: US20160083332A1
Автор: Knauf Thomas, Mairata Antoni
Принадлежит:

The present invention relates to a continuously operated adiabatic process for the preparation of nitrobenzene by nitration of benzene with nitric acid and sulfuric acid, in which the dilute sulfuric acid obtained after the nitration has taken place and the crude nitrobenzene has been separated off from the aqueous phase is concentrated for the purpose of re-use in the nitration, and after its concentration, at least one minute before it comes into contact with fresh nitric acid again an oxidizing agent is added such that a concentration of the oxidizing agent of from 10 ppm to 5,000 ppm, based on the total weight of the concentrated sulfuric acid to be recycled into the nitration, is established. 2. The process of claim 1 , wherein the oxidizing agent (c.2) is selected from the group consisting of nitric acid (c.2.1) claim 1 , nitrous acid (c.2.2) claim 1 , nitrosyisulfonic acid (c.2.3) and a mixture of at least two of these oxidizing agents.3. The process of claim 2 , wherein the oxidizing agent (c.2) is added 1 minute to 10 minutes before the phase (c.1) comprising sulfuric acid comes into contact with the nitric acid stream (a.3).4. The process of claim 2 , wherein the oxidizing agent (c.2) is added 3 minutes to 7 minutes before the phase (c.1) comprising sulfuric acid comes into contact with the nitric acid stream (a.3).5. The process of claim 1 , wherein a concentration of the oxidizing agent (c.2) of from 50 ppm to 2 claim 1 ,000 ppm claim 1 , based on the total weight of the concentrated aqueous phase (c.1) comprising sulfuric acid to be recycled into step a) claim 1 , is established.6. The process of claim 1 , wherein a concentration of the oxidizing agent (c.2) of from 100 ppm to 1 claim 1 ,000 ppm claim 1 , based on the total weight of the concentrated aqueous phase (c.1) comprising sulfuric acid to be recycled into step a) claim 1 , is established.7. The process of claim 1 , wherein the phase (c.1) comprising sulfuric acid is held ready in a sulfuric ...

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Номер записи: 84
31-03-2022 дата публикации

ARYL COMPOUNDS AND POLYMERS AND METHODS OF MAKING AND USING THE SAME

Номер: US20220098137A1
Автор: Chalifoux Wesley A., Sproul Kyle C., Yang Wenlong
Принадлежит: Nevada Research & Innovation Corporation

Disclosed herein are embodiments of aryl compounds and polymers thereof that are made using methods that do not require harsh conditions or expensive reagents. The methods disclosed herein utilize precursor compounds that can be polymerized to form polycyclic aromatic hydrocarbons and polymers, such as carbon-based polymers like nanostructures (e.g., graphene or graphene-like nanoribbons). 2. The compound of claim 1 , wherein the heteroaliphatic moiety comprises at least one carbon atom and one or two sulfur atoms.3. The compound of claim 1 , wherein each Rindependently is a thiol.4. The compound of claim 1 , wherein each Rindependently is a thioether.6. The compound of claim 5 , wherein the electron-donating group is an alkoxy group.9. The compound of claim 8 , wherein the electron-donating group is an alkoxy group. This application is a continuation of U.S. application Ser. No. 16/696,790, filed Nov. 26, 2019, which is a continuation of U.S. application Ser. No. 15/558,978, filed on Sep. 15, 2017, issued as U.S. Pat. No. 10,550,056 on Feb. 4, 2020, which is the U.S. National Stage of International Application No. PCT/US2016/023179, filed Mar. 18, 2016, which was published in English under PCT Article 21(2), which claims the benefit of, and priority to, the earlier filing date of U.S. Provisional Patent Application No. 62/135,692, filed on Mar. 19, 2015, and U.S. Provisional Patent Application No. 62/182,351, filed on Jun. 19, 2015; each of these prior applications is herein incorporated by reference in its entirety.The present disclosure concerns aryl compounds and polymeric aryl compounds and methods of making and using the same.Peropyrene compounds, as large polycyclic aromatic hydrocarbons (LPAH), comprise structural features that convey unique photophysical properties to such compounds. However, due to difficult preparation and derivatization of such compounds, their utility has yet to be utilized in various applications. Perylenediimide derivatives, which ...

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Номер записи: 85
12-06-2014 дата публикации

METHOD FOR PRODUCING NITROBENZENE COMPOUND

Номер: US20140163256A1
Автор: Hirano Yuuki, IDO TAKUYA, Ikumi Akiko, Tani Shinki, Yadomatsu Nami
Принадлежит: Ihara Chemical Industry Co., Ltd.

A method for producing a nitrobenzene compound represented by general formula (2), wherein Rand Rare the same or different, and each is a halogen atom or another functional group, and R, R, and Rare the same or different, and each is a hydrogen atom or another functional group, comprises oxidizing an aniline compound represented by general formula (1), wherein R, R, R, R, and Rare the same as described above, with hydrogen peroxide in the presence of a tungsten compound under an acidic condition, followed by oxidation with hydrogen peroxide under a neutral to alkaline condition. 122.-. (canceled)24. The method for producing a nitrobenzene compound according to claim 23 , wherein the oxidizing of the aniline compound represented by general formula (1) to the nitrobenzene compound represented by general formula (2) with the hydrogen peroxide is conducted by changing a pH condition in the oxidation reaction from an acidic condition to a neutral to alkaline condition.25. The method for producing a nitrobenzene compound according to claim 23 , wherein the oxidizing of the aniline compound to the nitrobenzene compound is conducted in the presence of a solvent.26. The method for producing a nitrobenzene compound according to claim 25 , wherein the solvent is water claim 25 , an alcohol claim 25 , a nitrile claim 25 , an aromatic hydrocarbon claim 25 , or a mixed solvent thereof.27. The method for producing a nitrobenzene compound according to claim 25 , wherein the solvent is water.28. The method for producing a nitrobenzene compound according to claim 25 , wherein the solvent is a mixed solvent of water and an aromatic hydrocarbon claim 25 , and the oxidizing of the aniline compound to the nitrobenzene compound is conducted in the presence of a phase transfer catalyst.29. The method for producing a nitrobenzene compound according to claim 28 , wherein the aromatic hydrocarbon is one or more selected from benzene claim 28 , chlorobenzene claim 28 , dichlorobenzene claim 28 ...

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Номер записи: 86
12-03-2020 дата публикации

Carbonate derivative production method

Номер: US20200079723A1
Автор: Akihiko Tsuda
Принадлежит: Kobe University NUC, Mitsubishi Gas Chemical Co Inc

The objective of the present invention is to provide a method for producing a carbonate derivative in a safe and efficient manner. The method for producing a carbonate derivative according to the present invention is characterized in comprising irradiating light on a composition containing a C1-4 halogenated hydrocarbon having one or more kinds of halogen atoms selected from the group consisting of a chlorine atom, a bromine atom and an iodine atom, a nucleophilic functional group-containing compound and the specific base in the presence of oxygen.

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Номер записи: 87
25-03-2021 дата публикации

PD(II)-CATALYZED ENANTIOSELECTIVE C-H ARYLATION OF FREE CARBOXYLIC ACIDS

Номер: US20210087131A1
Автор: Shen Peng-Xiang, YU JIN-QUAN
Принадлежит:

The invention includes procedures for stereoselective β-acylation of carboxylic acids having a β-carbon atom. For example, stereoselective acylation procedures include the following reactions: (I) 3. The method of wherein the Pd(II) salt is Pd(OAc).4. The method of wherein the carbonate base is NaCO claim 1 , or wherein the Ag(I) salt is AgCO claim 1 , or both.5. The method of wherein the Pd(II) salt is present at about 10 mole % claim 1 , the ligand is present at about 20 mole % claim 1 , or both.8. The method of wherein the Pd(II) salt is Pd(OAc).9. The method of wherein the carbonate base is NaCO claim 6 , or wherein the Ag(I) salt is AgCO claim 6 , or both.10. The method of wherein the Pd(II) salt is present at about 10 mole % claim 6 , the ligand is present at about 20 mole % claim 6 , or both. This application claims the priority of U.S. provisional application Ser. No. 62/659,866, filed Apr. 19, 2018, the disclosure of which is incorporated by reference herein in its entirety.This invention was made with government support under grant number GM084019 awarded by the National Institutes of Health. The government has certain rights in the invention.Desymmetrization through C—H activation holds the potential to become a broadly useful chiral technology due to the widespread presence of symmetric prochiral C(sp)—H bonds in the majority of organic molecules.Pd(II)-catalyzed enantioselective intermolecular C(sp)—H activation was recently made possible by a combination of weakly coordinating directing group and chiral bidentate ligand.This strategy was firstly demonstrated by the development of N-perfluoroaryl amide-directed enantioselective C—H cross-coupling of α-quaternary cyclopropanecarboxamides using mono-N-protected amino acids (MPAA) as the chiral ligands.Recently, chiral bidentate quinoline ligands were developed to realize enantioselective functionalization of methylene C(sp)—H bond of acyclic N-perfluoroaryl carboxamides to construct β-chiral centers,while ...

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Номер записи: 88
25-03-2021 дата публикации

SELECTIVE INHIBITORS OF NLRP3 INFLAMMASOME

Номер: US20210087147A1
Автор: BOCK Mark G., Boutard Nicolas Felix Pierre, Fabritius Charles-Henry Robert Yves, HARRISON David, LEVENETS Oleksandr, Porter Roderick Alan, TOPOLNICKI Grzegorz Witold, WATT Alan Paul
Принадлежит:

The present disclosure relates to compounds of Formula (I): 2. The compound of claim 1 , wherein Ris C-Cmonocyclic cycloalkyl claim 1 , polycyclic cycloalkyl claim 1 , or C-Caryl claim 1 , wherein the C-Cmonocyclic cycloalkyl claim 1 , polycyclic cycloalkyl claim 1 , or C-Caryl is optionally substituted by one or more R.3. The compound of or claim 1 , wherein Ris C-Cmonocyclic cycloalkyl optionally substituted by one or more R.4. The compound of any one of - claim 1 , wherein Ris cyclopentyl claim 1 , cyclohexyl claim 1 , or cycloheptyl claim 1 , wherein the cyclopentyl claim 1 , cyclohexyl claim 1 , or cycloheptyl is optionally substituted by one or more R.5. The compound of or claim 1 , wherein Ris C-Cpolycyclic cycloalkyl substituted by one or more R.6. The compound of any one of - and claim 1 , wherein Ris adamantly claim 1 , norbornyl claim 1 , or bicyclo[2.2.2]octanyl claim 1 , wherein the adamantly claim 1 , norbornyl claim 1 , or bicyclo[2.2.2]octanyl is optionally substituted by one or more R.7. The compound of any one of - and claim 1 , wherein Ris C-Ctricyclic saturated cycloalkyl optionally substituted by one or more R.8. The compound of any one of - claim 1 , claim 1 , and claim 1 , wherein Ris hexahydroindacenyl optionally substituted by one or more R.9. The compound of any one of - claim 1 , claim 1 , and - claim 1 , wherein Ris hexahydroindacenyl optionally substituted by one claim 1 , two claim 1 , three claim 1 , or four substituents independently selected from C-Calkyl claim 1 , C-Calkoxy claim 1 , halo claim 1 , oxo claim 1 , —OH claim 1 , and —CF.10. The compound of any one of - claim 1 , claim 1 , and - claim 1 , wherein Ris hexahydroindacenyl.13. The compound of or claim 1 , wherein Ris C-Caryl optionally substituted by one or more R.14. The compound of any one of - and claim 1 , wherein Ris phenyl optionally substituted by one or more R.15. The compound of any one of - and - claim 1 , wherein phenyl optionally substituted by one claim 1 , two ...

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Номер записи: 89
30-03-2017 дата публикации

Pharmaceutical compositions comprising monoterpenes

Номер: US20170088494A1
Автор: Thomas Chen
Принадлежит: Neonc Technologies Inc

The present invention provides a process for purifying a monoterpene or sesquiterpene having a purity greater than about 98.5% (w/w). The process comprises the steps of derivatizing the monoterpene (or sesquiterpene) to produce a monoterpene (or sesquiterpene) derivative, separating the monoterpene (or sesquiterpene) derivative, and releasing the monoterpene (or sesquiterpene) from the derivative. Also encompassed by the scope of the present invention is a pharmaceutical composition comprising a monoterpene (or sesquiterpene) having a purity greater than about 98.5% (w/w). The purified monoterpene can be used to treat a disease such as cancer. The present monoterpene (or sesquiterpene) may be administered alone, or may be co-administered with radiation or other therapeutic agents, such as chemotherapeutic agents.

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Номер записи: 90
02-04-2015 дата публикации

PROCESS FOR PREPARING N-(5-CHLORO-2-ISOPROPYLBENZYL)CYCLOPROPANAMINE

Номер: US20150094492A1
Автор: Himmler Thomas, LEHMANN Sandra, Müller Thomas Norbert, Riedrich Mathias, Rodefeld Lars, Volz Frank, VON MORGENSTERN Sascha
Принадлежит:

The present invention relates to a process for preparing N-(5-chloro-2-isopropylbenzyl)cyclopropanamine by hydrogenation of N-[(5-chloro-2-isopropylphenyl)methylene]cyclopropanamine over specific platinum catalysts. 12. The process according to wherein the acid used in step (g) to convert 3-bromo-4-isopropylaniline of the formula (VII) into the ammonium salts of the formula (VIII) is selected from the group consisting of HSO claim 9 , HCl claim 9 , HCOH claim 9 , HPO. The present invention relates to a process for preparing N-(5-chloro-2-isopropylbenzyl)cyclopropanamine by hydrogenation of N-[(5-chloro-2-isopropylphenyl)methylene]cyclopropanamine over specific platinum catalysts.Preparative processes for brominating strongly deactivated aromatics such as p-alkyl-substituted nitrobenzenes or nitrobenzene itself are described in the literature. The bromination of p-nitroethylbenzene by means of iron and bromine has been described with very low yields (55% yield of crude product and 34% after distillation) and with long reaction times of over 24 hours (1950, 72, 2804). The bromination of nitrobenzene by means of iron and bromine is described with a yield of always 60-75% of isolated compound (cf. 1941, Coll. Vol. I, 123, ibid. 1928, Vol 8, 48). A further possible way of brominating deactivated aromatics by means of potassium bromate is known (1981, 46, 2169-2171). However, reactions are problematical from a safety point of view because of the decomposition of potassium bromate in over 70% strength sulphuric acid solution. Furthermore, the bromination of p-nitrotoluene or nitrobenzene by means of N-bromosuccinimide in half-concentrated sulphuric acid is known (2006, 8, 645-6471965, 30, 304-306). However, this reaction requires N-bromosuccinimide as brominating reagent. Dimethyldibromohydantoin is found to be significantly more efficient (cf. 1994, 67, 1918-1921). However, trifluoromethanesulphonic acid, a very expensive reagent, is used here as proton source, which ...

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Номер записи: 91
02-04-2015 дата публикации

Process for the Manufacture of Nitropropanes

Номер: US20150094501A1
Автор: James Richard L., Trauth Daniel M.
Принадлежит:

Provided is a process for the formation of 2-nitropropane and/or 2,2-dinitropropane by the nitration of propane with dilute nitric acid. 111-. (canceled)12. An oil-based product stream directly obtained from a propane nitration reaction , comprising: 2-nitropropane; nitromethane; nitroethane; 1-nitropropane; and 2 ,2-dinitropropane , wherein the weight ratio of 2-nitropropane to 2 ,2-dinitropropane is at least about 15:1.13. A product stream according to wherein the weight ratio of 2-nitropropane to 2 claim 12 ,2-dinitropropane in the product stream is at least about 30:1.1418-. (canceled) This application claims the benefit of U.S. Provisional Application No. 61/045,378 filed Apr. 16, 2008.The invention relates to a process for making nitropropanes, such as 2-nitropropane and 2,2-dinitropropane. More specifically, the process comprises reacting aqueous nitric acid with propane under specific reaction conditions.The nitration of hydrocarbons generally produces a variety of products depending upon the reaction conditions and the feedstock structure. For instance, the commercial vapor phase process for propane nitration results in a mixture of four nitroparaffin products (nitromethane, 1-nitropropane, 2-nitropropane, and nitroethane) in essentially fixed relative concentrations.Certain products, however, may be more desirable than others and it has been a long-time goal to selectively produce the more useful nitrated compounds at the expense of the less useful compounds. In contrast to commercial vapor phase nitration, the mixed vapor-liquid phase or high pressure nitration of propane has been postulated in the past to be a technique by which 2-nitropropane, a more desirable nitroparaffin, can be potentially produced without making the other nitro compounds typically formed during vapor-phase nitration. See e.g., U.S. Pat. No. 2,489,320 (Nygaard et al.) and Albright, L. F., “Nitration of Paraffins”, Chem. Engr., (1966) pp. 149-156.The prior art technology for ...

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Номер записи: 92
05-05-2022 дата публикации

Process of Fluorinating Inorganic Compounds by Direct Fluorination

Номер: US20220135516A1
Автор: DU Hongjun, Wu Wenting, Zhou Changyue
Принадлежит: Fujian Yongjing Technology Co.,Ltd

The invention relates to a use of a fluorination gas, and the elemental fluorine (F) is present in a high concentration, for example, in a concentration of elemental fluorine (F), especially of equal to much higher than 15 or even 20% by volume, and to a process for the manufacture of a fluorinated compound by direct fluorination employing a fluorination gas, wherein the elemental fluorine (F) is present in a high concentration. The process of the invention is directed to the manufacture of a fluorinated compound, for the exception of fluorinated benzene, by direct fluorination. Especially the invention is of interest in the preparation of fluorinated organic compounds, final products and as well intermediates, for usage in agro-, pharma-, electronics-, catalyst, solvent and other functional chemical applications. The fluorination process of the invention may be performed batch-wise or in a continuous manner.

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Номер записи: 93
09-04-2015 дата публикации

METHOD FOR THE CONTINUOUS PRODUCTION OF NITROBENZENE

Номер: US20150099906A1
Автор: Knauf Thomas, Munnig Jurgen, Schmiedler Joerg
Принадлежит:

The present invention relates to a method for producing nitrobenzene, in which the waste gas streams accruing in the process and containing benzene and (traces of) nitrobenzene, possibly low- and medium-boiling components, possibly non-condensable gases and possibly water, optionally after removal of nitrogen oxides, are scrubbed in an absorption column with nitrobenzene, which comprises only very small amounts (maximum 50 ppm) of benzene and is distributed by means of a liquid distributor at a rate of 50 to 200 drip points per square metre, preferably 60 to 120 drip points per square metre, wherein (i) a liquid stream containing benzene and nitrobenzene, possibly organic low- and medium-boiling components and additionally containing sulfuric acid if sulfuric acid is used as the scrubbing agent and (ii) waste gas depleted in benzene and possibly in organic low- and medium-boiling components are obtained. A waste gas purified by the method according to the invention is particularly suitable for burning in a thermal exhaust air treatment process. 2. Method according to claim 1 , wherein step d) is performed under an absolute pressure of about 900 mbar to about 980 mbar.3. Method according to one of or claim 1 , wherein purified nitrobenzene from step c) is used as the scrubbing solution in step d).4. Method according to claim 3 , wherein the distillation in step c) is operated under an absolute pressure at the top of the distillation column of about 220 mbar to about 480 mbar and at a temperature at the bottom of the distillation column of about 100° C. to about 200° C.5. Method according to claim 3 , wherein the distillation in step c) is operated under an absolute pressure at the top of the distillation column of about 270 mbar to about 430 mbar and at a temperature at the bottom of the distillation column of about 120° C. to about 190° C. claim 3 , and wherein the purified nitrobenzene used as the scrubbing solution in step d) has a benzene content of <20 ppm claim ...

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Номер записи: 94
14-04-2016 дата публикации

Highly z-selective and enantioselective ring opening/cross metathesis catalyzed by a resolved stereogenic-at-ru complex

Номер: US20160101414A1
Автор: John Hartung, Robert H. Grubbs
Принадлежит: California Institute of Technology CalTech

This invention relates generally to enantiomerically enriched C—H activated ruthenium olefin metathesis catalyst compounds which are stereogenic at ruthenium, to the preparation of such compounds, and the use of such catalysts in the metathesis of olefins and olefin compounds, more particularly, in the use of such catalysts in enantio- and Z-selective olefin metathesis reactions. The invention has utility in the fields of catalysis, organic synthesis, polymer chemistry, and industrial and fine chemicals chemistry.

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Номер записи: 95
26-06-2014 дата публикации

EPOXIDATION OF GLYCEROL AND DERIVATIVES THEREFROM

Номер: US20140179936A1
Автор: Pienaar Andre, Stockenhuber Michael, Wilson Laurence Justin Pienaar
Принадлежит:

A method producing a surfactant from glycerol by converting glycerol, in a first step, to glycidol, polymerizing glycidol to an aliphatic alcohol and finally substituting a hydroxyl group with a substitute anion. 1. A method of producing a surfactant from glycerol which includes the steps of:(a) converting glycerol to glycidol;{'sub': n', '(2n+2), '(b) polymerizing glycidol to produce an aliphatic alcohol with a molecular formula CHOy, wherein n and y are numerical integers with n in the range 3 to 30 and y=n−1; and'}(c) substituting the hydroxyl moiety of the alcohol with a suitable head group.2. The method according to claim 1 , wherein the conversion of glycerol to glycidol includes the steps of dehydrating glycerol to acrolein (propenal) claim 1 , hydrogenating acrolein to allyl alcohol and epoxidizing allyl alcohol claim 1 , with hydrogen peroxide claim 1 , to glycidol.3. The method according to claim 2 , wherein a zeolite based catalyst is used in the dehydration step.4. The method according to claim 2 , wherein a hydrogenating catalyst claim 2 , including a support and at least one transition metal on the support claim 2 , is used in the hydrogenation step.5. The method according to claim 4 , wherein the at least one transition metal is cadmium claim 4 , silver or iron.6. The method according to claim 2 , wherein an epoxidizing catalyst claim 2 , being a titanium molecular sieve or a gold containing catalyst claim 2 , is used in the epoxidizing step.7. The method according to claim 1 , wherein polymerization claim 1 , in step (b) claim 1 , takes place by heating glycidol claim 1 , in an acidic medium claim 1 , for a predetermined period claim 1 , the length of which is dependent upon the number of carbon atoms (n) required in a tail group of the surfactant.8. The method according to claim 7 , wherein the polymerization step is initiated with boron trifluoride.9. The method according to claim 7 , wherein the tail group has a length in a range n=10 to 20.10. ...

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Номер записи: 96
16-04-2015 дата публикации

Point of use generation of amyl nitrite

Номер: US20150105475A1
Автор: Darrel W. Johnston, Joseph A. Mcdonough, Paul M. Thompson
Принадлежит: Southwest Research Institute SwRI

The present disclosure relates to devices and methods for the preparation of amyl nitrite formulations at a point of use location from relatively shelf-stable reagents employing acidic cationic exchange resins.

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Номер записи: 97
08-04-2021 дата публикации

C-ABL TYROSINE KINASE INHIBITORY COMPOUND EMBODIMENTS AND METHODS OF MAKING AND USING THE SAME

Номер: US20210101872A1
Автор: Alvarez Alejandra, Dextras Christopher R., Dulcey Andres E., Ferrer Marc, HU Xin, Marugan Juan J., Southall Noel T., Talley Daniel C., Von Bernhardi Rommy M., Zanlungo Silvana
Принадлежит:

Disclosed herein are embodiments of a compound that inhibits c-Abl tyrosine kinase (also referred to herein as “c-Abl”). The compound embodiments described herein are novel c-Abl inhibitors that can bind to c-Abl at an allosteric site and inhibit its activity in various pathways. The compound embodiments also are capable of crossing the blood brain barrier and therefore are useful in inhibiting c-Abl activity as it affects pathways and/or proteins in the brain. The compound embodiments described herein are effective therapeutic agents for treating diseases involving c-Abl, such as cancers, motor neuron diseases, and neurodegenerative diseases. Also disclosed herein are embodiments of methods for making and using the c-Abl inhibitory compound embodiments. 3. The compound of claim 1 , wherein each R′ and R″ independently is hydrogen claim 1 , alkyl claim 1 , alkenyl claim 1 , alkynyl claim 1 , aryl claim 1 , heteroalkyl claim 1 , heteroalkenyl claim 1 , heteroalkynyl claim 1 , heteroaryl claim 1 , alkyl-aryl claim 1 , alkenyl-aryl claim 1 , alkynyl-aryl claim 1 , alkyl-heteroaryl claim 1 , alkenyl-heteroaryl claim 1 , or alkynyl-heteroaryl.4. (canceled)5. The compound of claim 1 , wherein p is 1 and Ris hydrogen claim 1 , alkyl claim 1 , or heteroalkyl.6. The compound of claim 1 , wherein p is 1 and Ris hydrogen claim 1 , CH claim 1 , or —(CH)O(CH)Si(CH) claim 1 , wherein each q independently is an integer ranging from 0 to 50.7. The compound of claim 1 , wherein n is 1 and m is 1; or n is 0 and m is 1; or n is 1 and m is 0.89-. (canceled)10. The compound of claim 1 , wherein Y is oxygen claim 1 , NH claim 1 , NCH claim 1 , CH claim 1 , or C(CH)and Y is bound via a double bond; or wherein Y is hydrogen claim 1 , NH claim 1 , NHCH claim 1 , or N(CH)and Y is bound via a single bond.1112-. (canceled)13. The compound of claim 1 , wherein Rand Rindependently are alkoxy claim 1 , thioether claim 1 , haloalkoxy claim 1 , haloalkyl claim 1 , haloalkenyl claim 1 , haloalkynyl ...

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Номер записи: 98
13-04-2017 дата публикации

TRIPHASIC FLOW MILLIREACTORS

Номер: US20170101358A1
Автор: Khan Saif A., Yan Ning, Yap Swee Kun, Yuan Yuan
Принадлежит:

Disclosed is a reactor system that contains multiple millireactors, each including a millitube, a first feed line, a second feed line, and a third feed line. Each of the first and second feed lines has a hydraulic damper disposed therein. Also disclosed is a process for conducting in a millitube a triphasic flow reaction that requires a liquid reactant, a gas reactant, and a catalyst. 2. The reactor system of claim 1 , further comprising:a first liquid container connected to the first end of the first feed line, the first container connected in fluid communication to a first pump;a second liquid container connected to the first end of the second feed line, the second container connected in fluid communication to a second pump;a gas container connected to the first end of the third feed line; andan outflow container connected to the second end of the millitube.3. The reactor system of claim 2 , wherein the first and second pumps are each a peristaltic pump.4. The reactor system of claim 1 , wherein the millitube is a polytetrafluoroethylene tube.5. The reactor system of claim 4 , wherein the millitube has a length of 2-20 m and an inner diameter of 1-5 mm.6. The reactor system of claim 4 , wherein the first and second hydraulic dampers each consist of a first tube claim 4 , a second tube claim 4 , and a third tube in series claim 4 , the second tube having an inner diameter larger than that of the first tube and that of the third tube.7. The reactor system of claim 6 , wherein the first tube has the same length and inner diameter as those of the third tube.8. The reactor system of claim 6 , wherein the second tube in the first hydraulic damper is a silicone tube and the second tube in the second hydraulic damper is a viton tube.9. The reactor system of claim 5 , wherein the first and second hydraulic dampers each consist of a first tube claim 5 , a second tube claim 5 , and a third tube in series claim 5 , the second tube in each of the hydraulic dampers having an ...

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Номер записи: 99
13-04-2017 дата публикации

PROCESS FOR MAKING DI-FUNCTIONAL MOLECULES WITH CONCURRENT LIGHT PARAFFIN UPGRADING

Номер: US20170101366A1
Автор: Wang Kun
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An integrated process for making di-functional or multi-functional molecules with concurrent light paraffin upgrading is disclosed. The process involves three primary steps: (1) oxidation of an iso-paraffin to alkyl hydroperoxide and alcohol; (2) converting the alkyl hydroperoxide and alcohol to dialkyl peroxide; and (3) coupling functional molecules into di-functional or multi-functional molecules using the dialkyl peroxide as a radical initiator, while the dialkyl peroxide is converted to a tertiary alcohol. The functional molecules include any functional molecule R—X, where R is a hydrocarbyl group and X is a functional group such as —OH, —CN, —C(O)OH, —NH—, or the like. 1. A process for making di-functional or multi-functional molecules , comprising:(a) oxidizing a first feed stream comprising one or more iso-paraffins to form alkyl hydroperoxides and first tertiary alcohols;(b) catalytically converting the alkyl hydroperoxides and first alcohols to dialkyl peroxides; and(c) coupling a second feed stream using the dialkyl peroxides as a radical initiator to create di-functional or multi-functional molecules, while the dialkyl peroxides are converted to second tertiary alcohols.2. The process of claim 1 , wherein the first feed stream comprises iso-butane.3. The process of claim 1 , wherein the second feed stream comprises one or more functional molecules of the formula R—(CH)—CHXY; wherein —X and —Y are independently selected functional groups; wherein R is selected from hydrogen claim 1 , hydrocarbyl claim 1 , or an independently selected functional group; and wherein n is an integer in the range of 0-30.4. The process of claim 3 , wherein the one or more functional groups are independently selected from halogens claim 3 , —OH claim 3 , —CN claim 3 , —C(O)OH claim 3 , —NH— claim 3 , —SH claim 3 , —NO claim 3 , —OSOH claim 3 , —OPOH claim 3 , or —OBOH.5. The process of claim 4 , wherein the halogens are selected from —F claim 4 , —Cl claim 4 , —Br claim 4 , or — ...

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Номер записи: 100