СПОСОБ ОЧИСТКИ МЕЗОТРИОНА

FIELD: chemistry. ^ SUBSTANCE: method of purifying mesotrione involves preparing a solution of a mesotrione sample in a hydrogen-containing solvent, bringing pH of the solution to 9.5 or higher and crystallisation of mesotrione from the solution. ^ EFFECT: reduction of content of impurities in the mesotrione sample to an acceptable level. ^ 8 cl, 6 tbl, 6 ex РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) 2 373 193 (13) C2 (51) МПК C07C 315/06 C07C 317/24 (2006.01) (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ, ПАТЕНТАМ И ТОВАРНЫМ ЗНАКАМ (12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ (21), (22) Заявка: 2006137659/04, 03.03.2005 (24) Дата начала отсчета срока действия патента: 03.03.2005 (72) Автор(ы): БЕНКЕ Алан Хенри (US), УИЧЕРТ Джулия Мария (US) (43) Дата публикации заявки: 10.05.2008 2 3 7 3 1 9 3 (45) Опубликовано: 20.11.2009 Бюл. № 32 (56) Список документов, цитированных в отчете о поиске: US 4695673, 22.09.1987. US 6218579 B1, 17.04.2001. (85) Дата перевода заявки PCT на национальную фазу: 26.10.2006 2 3 7 3 1 9 3 R U (87) Публикация PCT: WO 2005/092846 (06.10.2005) C 2 C 2 (86) Заявка PCT: EP 2005/002230 (03.03.2005) Адрес для переписки: 101000, Москва, М.Златоустинский пер., 10, кв.15, "ЕВРОМАРКПАТ", пат.пов. И.А.Веселицкой, рег. № 11 (54) СПОСОБ ОЧИСТКИ МЕЗОТРИОНА (57) Реферат: Настоящее изобретение относится к способу очистки мезотриона, состоящему в приготовлении раствора образца мезотриона в водосодержащем растворителе, установлении pH указанного раствора равным 9,5 или выше и кристаллизации мезотриона из раствора. Настоящий способ позволяет снизить содержание примеси цианида в образце мезотриона до приемлемого уровня. 7 з.п. ф-лы, 6 табл. Ñòð.: 1 ru R U (73) Патентообладатель(и): ЗИНГЕНТА ПАРТИСИПЕЙШНС АГ (CH) (30) Конвенционный приоритет: 26.03.2004 GB 0406894.6 RUSSIAN FEDERATION (19) RU (11) 2 373 193 (13) C2 (51) Int. Cl. C07C 315/06 C07C 317/24 (2006.01) (2006.01) FEDERAL SERVICE FOR INTELLECTUAL PROPERTY, PATENTS AND TRADEMARKS (12) ABSTRACT OF INVENTION ...

ПОЛУЧЕНИЕ И КРИСТАЛЛИЗАЦИЯ S-[2-[1-(2-ЭТИЛБУТИЛ) ЦИКЛОГЕКСИЛКАРБОНИЛАМИНО]-ФЕНИЛ]-2-МЕТИЛТИОПРОПИОНАТА

Изобретение относится к способу получения S-[2-[1-(2-этилбутил)циклогексилкарбониламино]-фенил]-2-метилтиопропионата формулы (I), который применим в качестве фармацевтически активного соединения. Способ включает реакцию соединения формулы (II) с изомасляным ангидридом и восстановительным реагентом. Способ позволяет получать S-[2-[1-(2-этилбутил)циклогексилкарбониламино]-фенил]-2-метилтиопропионата с более высоким выходом продукта. 9 з.п. ф-лы, 12 пр.

Electrodialysis-distillation hybrid process for the recovery of dimethylsulfoxide (DMSO) solvent from industrial effluent

Process for purification of dimethyl sulphoxide (DMSO)

PRODUCTION OF AROMATIC SULPHONES

PROCEDURE FOR AUFREINIGUNG OF MESOTRION

PROCEDURE FOR THE PRODUCTION OF BICALUTAMID AND PROCEDURES FOR AUFREINIGUNG OF INTERMEDIATE PRODUCTS FOR IT

PROCEDURE FOR THE CLEANING OF DIMETHYLSULFOXID (DMSO)

4-hydroxy-4'-isopropoxydiphenyl sulfone developer composition, wet pulverizing method, and dispersion

ORGANIC-SULPHIDE COMPOSITION WITH MASKED ODOUR

La présente invention concerne le masquage d'odeur des sulfures organiques et plus particulièrement celui des sulfures d'alkyle ou de dialkyle, notamment du sulfure de diméthyle, ainsi que de leurs oxydes, et notamment du diméthylsulfoxyde, par addition auxdits sulfures organiques d'au moins un agent masquant d'odeur comprenant au moins un mono-ester, au moins un di- ou tri- ester, au moins un alcool, au moins une cétone et éventuellement au moins un terpène.

PROCESS FOR PREPARATION OF BICALUTAMIDE

PROCESS FOR PURIFYING AND ISOLATING RAC-BICALUTAMIDE

The present invention discloses a new process for the isolation and purification of racemic and optically active bicalutamide.

PROCESS FOR PREPARING BENZHYDRYLTHIOACETAMIDE

The present invention is directed to an improved process for preparing modafinil wherein benzhydrylthioacetamide is prepared in high yield and purity by the reaction of a haloacetamide with the reaction product of thiourea and benzhydrol in aqueous solution. The reaction employing the haloacetamide is conducted in a solvent comprising water and an organic solvent such as dimethylformamide having dissolved therein a basic salt such as potassium carbonate. The resulting benzhydrylthioacetamide can be oxidized to provide the pharmaceutical modafinil.

PROCESS FOR PREPARING 3-METHYLSULFONYLPROPIONITRILE

The present invention relates to processes for preparing 3-methylsulfonylpropionitrile. The processes provide a good yield and a good purity of the final product and provide a controllable reaction. The present invention also relates to a crystalline form of 3- methylsulfonylpropionitrile having X-ray diffraction peaks at 13.9 ± 0.1, 19.2± 0.1, 20.0± 0.1, 22.5± 0.1, 23.2± 0.1, 25.7± 0.1, 28.1± 0.1, 29.9± 0.1, and 30.6± 0.1 degrees 20, and wherein the most intense peak is the peak at 13.9 ± 0.1 degrees 20.

STEREOISOMERIC ENRICHMENT OF 2-AMINO-3-HYDROXY-3-PHENYLPROPIONIC ACIDS

Mixtures of enantiomeric D,L-threo 2-amino-3-hydroxy-3- phenylpropionic acids can be stereoisomerically enriched by contacting the mixture with a D-threonine aldolase. In a typical embodiment, D- and L-threo 2-amino-3-hydroxy-3-(4- methylsulfonylphenyl)propionic acid is treated with D-threo- nine aldolase to produce L-threo 2-amino-3-hydroxy-3-(4- methylsulfonylphenyl)propionic acid with a high ee. The benzaldehyde and amino acid formed from the D-threo isomer can be recycled.

КОМПОЗИЦИЯ НА ОСНОВЕ ОРГАНИЧЕСКОГО СУЛЬФИДА С ЗАМАСКИРОВАННЫМ ЗАПАХОМ

Данное изобретение относится к области маскировки запаха органических сульфидов, более конкретно сульфидов алкила или диалкила, в частности диметилсульфида, а также их оксидов, в частности диметилсульфоксида, путем добавления к указанным органическим сульфидам, по меньшей мере, одного маскирующего запах агента, который содержит, по меньшей мере, один сложный моноэфир, по меньшей мере один сложный ди- и/или триэфир, по меньшей мере один спирт, по меньшей мере один кетон и возможно по меньшей мере один терпен.

СПОСІБЗНИЖЕННЯ ВМІСТУ ЦІАНІДУ В ЗРАЗКУ МЕЗОТРІОНУ

У заявці описаний спосіб зниження вмісту ціаніду в зразку мезотріону. Зазначений спосіб включає: (і) приготування водного розчину зразка мезотріону у водному розчиннику, (іі) встановлення рН зазначеного водного розчину на значення 9,5 або вище, та (ііі) кристалізацію мезотріону з розчину.

CRYSTALLINE AND PURE MODAFINIL, AND PROCESS OF PREPARING THE SAME

The present invention provides an improved process for preparing modafinil, whereby it may be isolated in high purity by a single crystallization. The process produces modafinil free of sulphone products of over-oxidation and other byproducts. The invention further provides new crystalline Forms II-VI of modafinil and processes for preparing them. Each of the new forms is differentiated by a unique powder X-ray diffraction pattern. The invention further provides pharmaceutical compositions containing novel modafinil Forms II-IV and VI. © KIPO & WIPO 2007 ...

Process for distilling dimethyl, sulfoxide and multistage distillation column

process for the purification of mesotrione

Process for the extractive removal of phospho- and sulfobetaines from acidic reaction solutions

The ampholytes are extracted from the reaction solution with a liquid cation exchanger which is immiscible with the acidic aqueous reaction solution, where the cation exchanger is dissolved in at least one organic solvent which is immiscible with water and forms an organic phase with the organic solvent. Subsequently the organic phase which is loaded with the ampholyte is separated from the reaction solution, and then the ampholytes are back-extracted from the organic phase with aqueous solvents. The product losses in the process are low, and the residual salt content is very low.

PROCESS FOR PURIFYING MESOTRIONE

PROCESS FOR WORKING UP A COMPOSITION COMPRISING SOLID 4,4'-DICHLORODIPHENYL SULFOXIDE AND A SOLVENT

METHOD FOR PRODUCING 2,4'-DIHYDROXYDIPHENYL SULFONE

PROBLEM TO BE SOLVED: To provide a method for producing 2,4'-dihydroxydiphenyl sulfone (2,4'-DDS), capable of economically, advantageously, and efficiently separating the 2,4'-DDS from a reaction mixture containing 4,4'-dihydroxydiphenyl sulfone (4,4'-DDS) and the 2,4'-DDS, and capable of effectively utilizing phenolsulfonic acid contained in the reaction mixture as a raw material. SOLUTION: In this method for producing the 2,4'-DDS, the 4,4'-DDS is separated through crystallization from a mixture which is obtained by dehydration reaction of phenol with sulfuric acid, or with the phenolsulfonic acid, and contains the 4,4'-DDS, the 2,4'-DDS, the phenolsulfonic acid, and the phenol, so as to obtain a mixture in which a content of the 2,4'-DDS is higher than that of the 4,4'-DDS, then the obtained mixture is controlled to have such a solvent composition that a weight ratio of the phenol to water is 10:90 to 90:10, so as to make the 2,4'-DDS crystallized, and further the crystallized 2,4'-DDS ...

СПОСОБ ОЧИСТКИ МЕЗОТРИОНА

... 1. Способ уменьшения содержания нежелательных примесей в образце мезотриона, заключающийся в том, что (I) готовят раствор енолята мезотриона в водосодержащем растворителе; (II) проводят одну или несколько стадий очистки и (III) кристаллизуют очищенный мезотрион из раствора. 2. Способ по п.1, который дополнительно включает стадию дистилляции. 3. Способ по п.1 или 2, в котором один или несколько процессов очистки выбирают из группы, включающей фильтрацию, адсорбцию, экстракцию органическим растворителем и декантацию. 4. Способ уменьшения содержания нежелательных примесей в образце мезотриона, заключающийся в том, что проводят стадию дистилляции, готовят раствор енолята мезотриона, выполняют одну или несколько стадий очистки и кристаллизуют мезотрион. 5. Способ уменьшения содержания нежелательных примесей в образце мезотриона, заключающийся в том, что готовят раствор енолята мезотриона, в произвольном порядке проводят декантацию, фильтрацию и адсорбцию и кристаллизуют мезотрион. 6. Объединенный ...

ПОЛУЧЕНИЕ И КРИСТАЛЛИЗАЦИЯ S-[2-[1-(2-ЭТИЛБУТИЛ) ЦИКЛОГЕКСИЛКАРБОНИЛАМИНО]-ФЕНИЛ]-2-МЕТИЛТИОПРОПИОНАТА

... 1. Способ получения соединения формулы (I):который включает реакцию соединения формулы (III)с изомасляным ангидридом и восстановительным реагентом.2. Способ по п.1, в котором ацилирование проводят с использованием не менее 0,10 М восстановительного реагента.3. Способ по п.1 или 2, в котором указанный восстановительный реагент представляет собой фосфин, фосфинит, фосфонит или фосфит.4. Способ по п.1, который дополнительно включает окисление избытка восстановительного реагента окислительным реагентом.5. Способ по п.4, в котором окислительный реагент представляет собой оксон® или пероксид водорода, наиболее предпочтительно, если окислительный реагент представляет собой пероксид водорода.6. Способ по п.1, в котором указанный восстановительный реагент представляет собой фосфин.7. Способ по п.1, в котором указанный восстановительный реагент представляет собой трифенилфосфин.8. Способ по п.1, который дополнительно включает экстракцию фосфиноксида, фосфината, фосфоната или фосфата из соединения ...

ОЧИСТКА 2-НИТРО-4-МЕТИЛСУЛЬФОНИЛБЕНЗОЙНОЙ КИСЛОТЫ

... 1. Способ удаления примесей из 2-нитро-4-метилсульфонилбензойной кислоты, включающий по меньшей мере две из следующих стадий, в любом порядке, (а) растворение 2-нитро-4-метилсульфонилбензойной кислоты в воде при рН примерно 2-10 с последующей фильтрацией; (b) контактирование водного раствора 2-нитро-4-метилсульфонилбензойной кислоты с активированным углем при рН примерно 2-10; (с) обработка водного раствора 2-нитро-4-метилсульфонилбензойной кислоты достаточным количеством основания для гидролиза нежелательных нитро- и динитрозамещенных примесей; с последующим выдерживанием полученного водного раствора, содержащего 2-нитро-4-метилсульфонилбензойную кислоту, при температуре вплоть до около 95°С и доведением рН указанного раствора до примерно рН, достаточного для осуществления кристаллизации 2-нитро-4-метилсульфонилбензойной кислоты при охлаждении. 2. Способ по п.1, в котором используют стадии (а) и (b). 3. Способ по п.1, в котором используют стадии (а) и (с). 4. Способ по п.1, в котором используют ...

Electrodialysis-distillation hybrid process for the recovery of dimethylsulfoxide (DMSO) solvent from industrial effluent

Process for purifying mesotrione

Process for isolating 4,4'-dihydroxydiphenyl sulfone from a mixture of dihydroxydiphenyl sulfone isomers

... 4,4 min -Dihydroxydiphenyl sulfone is isolated from a mixture of dihydroxydiphenyl sulfone isomers by heat dissolving the mixture in phenol and then cooling the resulting solution thereby allowing 4,4 min -dihydroxydiphenyl sulfone to precipitate as an adduct with phenol.

STEREOISOMERI ENRICHMENT OF 2-AMINO-3 HYDROXY-3-PHENYL-PROPIONSÄUREN

PROCEDURE FOR THE CRYSTALLIZATION OF BICALUTAMID

BICALUTAMIDKRISTALLE AND PROCEDURE FOR THEIR PRODUCTION

PROCEDURE FOR THE PRODUCTION OF MODAFINIL

PROCEDURE FOR the PRODUCTION OF 1,2-DISULFONVERBINDUNGEN.

PROCEDURE FOR THE CLEANING OF DIMETHYLSULFOXYD (DMSO)

Process for preparation of bicalutamide

Process for producing bicalutamide and method of purifying intermediate therefor

METHOD FOR THE PRODUCTION OF CRYSTALLINE FORMS AND CRYSTALLINE FORMS OF OPTICAL ENANTIOMERS OF MODAFINIL

L'invention a pour objet un procédé de préparation de formes cristallines des énantiomères optiques du modafinil, comprenant les étapes consistant à :i) dissoudre l'un des énantiomères optiques du modafinil dans un solvant autre que l'éthanol ;ii) cristalliser l'énantiomère du modafinil ;iii) récupérer la forme cristalline de l'énantiomère du modafinil ainsi obtenue.L'invention vise également un procédé de préparation des énantiomères optiques du modafinil.

HIGH PURITY DIPHENYL SULFONE, PREPARATION AND USE THEREOF FOR THE PREPARATION OF A POLY(ARYLETHERKETONE)

The presence of certain impurities in diphenyl sulfone have a deleterious effect on the properties of the poly(aryletherketone)s produced therein, including one or more of color, melt stability, molecular weight, crystallinity, etc. and here identify those impurities and provide processes for the removal of such impurities.

IMPROVED PROCESS FOR PREPARING A POLY(ARYL ETHER KETONE) USING A HIGH PURITY 4,4'-DIFLUOROBENZOPHENONE

The present invention describes a process for preparing a poly(aryl ether ketone) by reacting a nucleophile with 4,4'-difluorobenzophenone (4,4'-DFBP) that is improved through the use of 4,4'-DFBP that meets one or more particular purity conditions. Also described are improved poly(aryl ether ketone) produced using the invention 4,4'-DFBP. Amounts of 2,4'-difluorobenzophenone (2,4'-DFBP), 4-monofluorobenzophenone (4-FBP), chlorine, and monochloromonofluorobenzophenone in 4,4'-DFBP are discussed.

ORGANIC-SULPHIDE COMPOSITION WITH MASKED ODOUR

La présente invention concerne le masquage d'odeur des sulfures organiques et plus particulièrement celui des sulfures d'alkyle ou de dialkyle, notamment du sulfure de diméthyle, ainsi que de leurs oxydes, et notamment du diméthylsulfoxyde, par addition auxdits sulfures organiques d'au moins un agent masquant d'odeur comprenant au moins un mono-ester, au moins un di- ou tri- ester, au moins un alcool, au moins une cétone et éventuellement au moins un terpène.

PROCESS FOR THE CRYSTALLISATION OF MESOTRIONE

The invention relates to a process for selectively controlling the crystallisation mesotrione [2-(4-methylsulphonyl-2-nitrobenzoyl)cyclohexane-1 ,3-dione] from aqueous solution in which the aqueous mesotrione solution is introduced to a crystalliser containing seed crystals predominantly of the thermodynamically stable polymorph ("Form 1") in a semi-continuous or continuous manner. The invention further relates to a process for converting the metastable polymorph ("Form 2") of mesotrione to Form 1 by introducing an aqueous solution containing the former form to a crystalliser containing seed crystals predominantly of the latter form.

CRYSTALLINE AND PURE MODAFINIL, AND PROCESS OF PREPARING THESAME

The present invention provides an improved process for preparing modafinil, whereby it may be isolated in high purity by a single crystallization. The process produces modafinil free of sulphone products of over-oxidation and other byproducts. The invention further provides new crystalline Forms II-VI of modafinil and processes for preparing them. Each of the new forms is differentiated by a unique powder X-ray diffraction pattern. The invention further provides pharmaceutical compositions containing novel modafinil Forms II-IV and VI.

PURIFICATION PROCESS OF 3,3'-DINITRODIPHENYL COMPOUNDS

CRYSTALLINE AND PURE MODAFINIL, AND PROCESS OF PREPARING THE SAME

The present invention provides an improved process for preparing modafinil, whereby it may be isolated in high purity by a single crystallization. The process produces modafinil free of sulphone products of over-oxidation and other byproducts. The invention further provides new crystalline Forms II-VI of modafinil and processes for preparing them. Each of the new forms is differentiated by a unique powder X-ray diffraction pattern. The invention further provides pharmaceutical compositions containing novel modafinil Forms II-IV and VI.

METHOD OF PREPARING MODAFINIL POLYMORPHIC FORM I

The present invention relates to a method of preparing CRL 40476 Form I of modafinil comprising slurrying or suspending a polymorphic form of modafinil or a solvate of modafinil in a solvent to obtain or to form a solution; and separating modafinil CRL 40476 form I from said solvent.

СПОСОБЫ ПОЛУЧЕНИЯ ПОЛИМОРФНЫХ ФОРМ МЕЗОТРИОНА И ПРИМЕНЕНИЕ РЕГУЛИРОВАНИЯ РН

В заявке описан способ селективного регулирования кристаллизации термодинамически стабильной формы 1 или кинетически стабильной полиморфной формы 2 мезотриона из водного раствора мезотриона, где указанный способ включает изменение рН раствора мезотриона до значения, при котором в конечном итоге образуют термодинамически стабильную форму 1 или кинетически стабильную форму 2 мезотриона. Также описан способ преобразования формы 2 мезотриона в форму 1 мезотриона. Кроме того, изобретение касается и применения регулирования рН до значения ≤ 2,5 для получения термодинамически стабильной формы 1 мезотриона.

СПОСОБ СЕЛЕКТИВНОГО РЕГУЛИРОВАНИЯ КРИСТАЛЛИЗАЦИИ ПОЛИМОРФНОЙ ФОРМЫ 1 МЕЗОТРИОНА

Данное изобретение относится к способу селективного регулирования кристаллизации полиморфных форм мезотриона. Данное изобретение также относится к использованию полунепрерывного или непрерывного способа для регулирования образования полиморфных форм.

СПОСІБ ВИЛУЧЕННЯ ДОМІШОК З 2-НІТРО-4-МЕТИЛСУЛЬФОНІЛБЕНЗОЙНОЇ КИСЛОТИ, ОЧИЩЕНА 2-НІТРО-4-МЕТИЛСУЛЬФОНІЛБЕНЗОЙНА КИСЛОТА ТА СПОСІБ ОДЕРЖАННЯ МЕЗОТРИОНУ

Cпосіб видалення домішок з 2-нітро-4-метилсульфонілбензойної кислоти, що включає такі стадії в будь-якому порядку: (а) розчинення 2-нітро-4-метилсульфонілбензойної кислоти у воді при pH приблизно 2-10 з подальшою фільтрацією; (b) контактування водного розчину 2-нітро-4-метилсульфонілбензойної кислоти з активованим вугіллям при pH приблизно 2-10; (с) обробка водного розчину 2-нітро-4-метилсульфонілбензойної кислоти достатньою кількістю основи для гідролізу небажаних нітро- і динітрозаміщених домішок.

СПОСОБ ПОЛУЧЕНИЯ КРИСТАЛЛИЧЕСКИХ ФОРМ И КРИСТАЛЛИЧЕСКИЕ ФОРМЫ ОПТИЧЕСКИХ ЭНАНТИОМЕРОВ МОДАФИНИЛА

Изобретение относится к способу получения кристаллических форм оптических энантиомеров модафинила, включающему в себя следующие этапы: i) растворение одного из оптических энантиомеров модафинила в растворителе, не являющемся этанолом; ii) кристаллизация энантиомера модафинила; iii) выделение полученной кристаллической формы энантиомера модафинила. Изобретение касается также способа получения оптических энантиомеров модафинила.

METHOD FOR SYNTHESIS OF CHIRAL PROPARGYL ALCOHOLS

СПОСОБ ПОЛУЧЕНИЯ КРИСТАЛЛИЧЕСКИХ ФОРМ И КРИСТАЛЛИЧЕСКИЕ ФОРМЫ ОПТИЧЕСКИХ ЭНАНТИОМЕРОВ МОДАФИНИЛА

Изобретение касается способа получения кристаллических форм оптических энантиомеров модафинила, включающего следующие этапы: и) растворение одного из оптических энантиомеров модафинила в растворителе, не являющимся этанолом; ii) кристаллизация энантиомера модафинила; iii) выделение полученной кристаллической формы энантиомера модафинила. Изобретение касается также способа получения оптических энантиомеров модафинила.

FORMULATION OF DIMETHYLSULFOXYDE IN MIXTURE WITH an ADDITIVE ALLOWING TO LOWER the POINT OF CRYSTALLIZATION OF THIS LAST, AND APPLICATIONS OF THIS MIXTURE

DIPHENYL SULPHONE DERIVATIVES

IMPROVED METHOD FOR PURIFYING SULFONATED AROMATIC MONOMER

PROCESS FOR THE PREPARATION OF POLYMORPHS OF MESOTRIONE

A process for selectively controlling the crystallisation of thermodynamically stable Form (1) or kinetically stable Form (2) polymorphs of mesotrione from an aqueous mesotrione solution, said method comprising adjusting the pH of the mesotrione solutions to a value wherein said thermodynamically stable Form (1) or kinetically stable Form (2) mesotrione is ultimately obtained is disclosed. © KIPO & WIPO 2007 ...

CRYSTALLINE AND PURE MODAFINIL, AND PROCESS OF PREPARING THE SAME

The present invention provides an improved process for preparing modafinil, whereby it may be isolated in high purity by a single crystallization. The process produces modafinil free of sulphone products of over-oxidation and other byproducts. The invention further provides new crystalline Forms II-VI of modafinil and processes for preparing them. Each of the new forms is differentiated by a unique powder X-ray diffraction pattern. The invention further provides pharmaceutical compositions containing novel modafinil Forms II-IV and VI. © KIPO & WIPO 2007 ...

PROCEDURE FOR THE PREPARATION OF ACID BETA-SULFATOETILSULFONILANILIN-2-SULFONICO

Procedimiento para la preparacion del ácido beta-sulfatoetilsulfonilanilin-2-sulfonico, que se encuentra como solucion en ácido sulfurico acuoso, en donde: en un primer paso se precipita el ácido beta-sulfatoetilsulfonilanilin-2-sulfonico por adicion de sales alcalinas(alcalinotérreas) y/o de amonio, se separa y se disuelve en agua, o se precipita el ácido sulfurico por adicion de sales de calcio, se separa eventualmente el sulfato de calcio obtenido; y en un segundo paso se ajusta el pH de la solucion obtenida por adicion de hidroxido, carbonato, hidrogenocarbonato y/o acetato alcalino(alcalinotérreo) o de amonio a un valor entre 1 y 5, se separa sulfato de calcio aun presente y se aísla el ácido beta-sulfatoetilsulfonilanilin-2- sulfonico de la solucion.

MODAFINIL POLYMORPHIC FORMS

The present invention relates to modafinil polymorphic forms, methods of preparation thereof, pharmaceutical compositions and methods of therapeutic treatment involving modafinil polymorphic forms.

Alkylation catalyst regeneration

Disclosed is a process for removing acid soluble oils, produced as an undesirable by-product of an HF (catalyzed alkylation reaction, from a fluid containing a sulfone compound. The process includes the use of hydrocarbons to remove ASO from the sulfone-containing fluid.

Process for preparing an organic sulfone

A process for preparing polyaryl ethers in which a polycondensation of the monomer building blocks is carried out using microwave irradiation leads to thermoplastic molding compositions having improved color properties.

CRYSTAL COMPOSITION (CC) COMPRISING 4,4'-DICHLORODIPHENYLSULFOXIDE CRYSTALS (C)

The invention relates to a crystal (C) consisting of at least 95% by weight of 4,4′-dichlorodiphenylsulfoxide, 0 to 2% by weight of impurities and 0 to 3% by weight of an organic solvent (os). Moreover, the present invention relates to a crystal composition (CC) comprising crystals (C) and a process for the production of the crystal composition (CC) and the crystal (C).

Crystalline and pure modafinil, and process of preparing the same

The present invention provides an improved process for preparing modafinil, whereby it may be isolated in high purity by a single crystallization. The process produces modafinil free of sulphone products of over-oxidation and other byproducts. The invention further provides new crystalline Forms II-VI of modafinil and processes for preparing them. Each of the new forms is differentiated by a unique powder X-ray diffraction pattern. The invention further provides pharmaceutical compositions containing novel modafinil Forms II-IV and VI.

4-HYDROXY-4'-ISOPROPOXYDIPHENYL SULFONE DEVELOPER COMPOSITION, WET PULVERIZING METHOD, AND DISPERSION

СПОСОБ ОЧИСТКИ МЕЗОТРИОНА

Настоящее изобретение относится к способу уменьшения содержания нежелательных примесей в мезотрионе, который применяют в качестве гербицида. Способ заключается в том, что 1) готовят раствор енолята мезотриона в водосодержащем растворителе; 2) проводят одну или несколько стадий очистки, выбранных из группы, включающей фильтрацию, адсорбцию, экстракцию органическим растворителем и декантацию, и 3) кристаллизуют мезотрион из раствора, полученного на стадии 2). Технический результат - разработка нового способа очистки мезотриона. 9 н. и 5 з.п. ф-лы, 12 табл.

УЛУЧШЕННЫЙ СПОСОБ ПРОИЗВОДСТВА ПОЛИ(АРИЛЭФИРКЕТОН)ОВ И УЛУЧШЕННЫЙ СПОСОБ СНАБЖЕНИЯ КАРБОНАТОМ НАТРИЯ, ПРИЕМЛЕМЫМ ДЛЯ ПРОИЗВОДСТВА ПОЛИ(АРИЛЭФИРКЕТОН)ОВ

... 1. Способ получения карбоната натрия, который особенно хорошо подходит для получения поли(арилэфиркетона) ароматическим нуклеофильным замещением, включающий:- синтез химически легкого карбоната натрия;- выявление из легкого карбоната натрия, по меньшей мере, одной партии, имеющей следующее распределение частиц по размерам:D≥45 мкм и D≤250 мкм и D≤710 мкм;- дифференцирование партии от остального легкого карбоната натрия;- получение, по меньшей мере, части партии.2. Способ по п.1, отличающийся тем, что легкий карбонат натрия химически синтезирован с помощью аммиачно-содового способа, общей реакционной схемой процесса которого является:2NaCl+CaCO→NaCO+CaCl.3. Способ по п.2, отличающийся тем, что аммиачно-содовый способ включает:- пропускание диоксида углерода (СО) через водный раствор хлорида натрия (NaCl) и аммиака (NH) так, чтобы получить осадок бикарбоната натрия (NaHCO) в соответствии со следующей схемой реакции:NaCl+CO+NH+HO→NaHCO+NHCl,- затем превращение осадка бикарбоната натрия (NaHCO ...

СПОСОБ ОЧИСТКИ МЕЗОТРИОНА

ÐÎÑÑÈÉÑÊÀß ÔÅÄÅÐÀÖÈß RU (19) (11) 2006 137 659 (13) A (51) ÌÏÊ C07C 315/06 (2006.01) ÔÅÄÅÐÀËÜÍÀß ÑËÓÆÁÀ ÏÎ ÈÍÒÅËËÅÊÒÓÀËÜÍÎÉ ÑÎÁÑÒÂÅÍÍÎÑÒÈ, ÏÀÒÅÍÒÀÌ È ÒÎÂÀÐÍÛÌ ÇÍÀÊÀÌ (12) ÇÀßÂÊÀ ÍÀ ÈÇÎÁÐÅÒÅÍÈÅ (21), (22) Çà âêà: 2006137659/04, 03.03.2005 (71) Çà âèòåëü(è): ÇÈÍÃÅÍÒÀ ÏÀÐÒÈÑÈÏÅÉØÍÑ Àà (CH) (30) Êîíâåíöèîííûé ïðèîðèòåò: 26.03.2004 GB 0406894.6 (43) Äàòà ïóáëèêàöèè çà âêè: 10.05.2008 Áþë. ¹ 13 (72) Àâòîð(û): ÁÅÍÊÅ Àëàí Õåíðè (US), ÓÈ×ÅÐÒ Äæóëè Ìàðè (US) (87) Ïóáëèêàöè PCT: WO 2005/092846 (06.10.2005) Àäðåñ äë ïåðåïèñêè: 101000, Ìîñêâà, Ìàëûé Çëàòîóñòèíñêèé ïåð., 10, êâ.15, "ÅÂÐÎÌÀÐÊÏÀÒ", ïàò.ïîâ. Í.Â.Êóçåíêîâîé R U (57) Ôîðìóëà èçîáðåòåíè 1. Ñïîñîá ñíèæåíè ñîäåðæàíè öèàíèäà â îáðàçöå ìåçîòðèîíà, óêàçàííûé ñïîñîá âêëþ÷àåò (i) ïðèãîòîâëåíèå âîäíîãî ðàñòâîðà îáðàçöà ìåçîòðèîíà â âîäíîì ðàñòâîðèòåëå, (ii) óñòàíîâëåíèå ðÍ óêàçàííîãî âîäíîãî ðàñòâîðà ðàâíûì 9,5 èëè âûøå, è (iii) êðèñòàëëèçàöèþ ìåçîòðèîíà èç ðàñòâîðà. 2. Ñïîñîá ïî ï.1, â êîòîðîì îáðàçåö ìåçîòðèîíà ïðåäâàðèòåëüíî âûäåë ëè è ïîâòîðíî ðàñòâîð ëè â âîäíîì ðàñòâîðèòåëå. 3. Ñïîñîá ïî ï.1, â êîòîðîì îáðàçåö ìåçîòðèîíà ïðåäâàðèòåëüíî íå âûäåë ëè è îí óæå ñîäåðæàëñ â âèäå âîäíîãî ðàñòâîðà â âîäíîì ðàñòâîðèòåëå. 4. Ñïîñîá ïî ï.3, êîòîðûé äîïîëíèòåëüíî âêëþ÷àåò ñòàäèþ îòãîíêè. 5. Ñïîñîá ïî ï.4, â êîòîðîì ñòàäèþ îòãîíêè ïðîâîä ò äî óñòàíîâëåíè çíà÷åíè ðÍ âîäíîãî ðàñòâîðà ðàâíûì 9,5 èëè âûøå. 6. Ñïîñîá ïî ï.4, â êîòîðîì ñòàäèþ îòãîíêè ïðîâîä ò ïîñëå óñòàíîâëåíè çíà÷åíè ðÍ âîäíîãî ðàñòâîðà ðàâíûì 9,5 èëè âûøå. 7. Ñïîñîá ïî ï.1, â êîòîðîì ñòàäè êðèñòàëëèçàöèè òàêæå âêëþ÷àåò ñòàäèþ ïðîäóâêè àçîòîì. 8. Ñïîñîá ïî ï.1, â êîòîðîì ñîäåðæàíèå öèàíèäà â îáðàçöå ìåçîòðèîíà ñíèæàåòñ äî ðàâíîãî 150 ìàñ.÷àñò./ìëí èëè ìåíåå. Ñòðàíèöà: 1 RU A 2 0 0 6 1 3 7 6 5 9 A (54) ÑÏÎÑÎÁ Î×ÈÑÒÊÈ ÌÅÇÎÒÐÈÎÍÀ 2 0 0 6 1 3 7 6 5 9 (86) Çà âêà PCT: EP 2005/002230 (03.03.2005) R U (85) Äàòà ïåðåâîäà çà âêè PCT íà íàöèîíàëüíóþ ôàçó: 26.10.2006

KRISTALLINES UND REINES MODAFINIL UND VERFAHREN ZU SEINER HERSTELLUNG

GEWINNUNG VON 4,4'-DICHLORDIPHENYLSULFON

Verfahren zur Reinigung von Dimethylsulfoxid (DMSO)

VERFAHREN ZUR HERSTELLUNG VON 1,2-DISULFON-VERBINDUNGEN.

CLEANING OF HALOGENIERTEN AROMATIC SULFONES AND KETONEN.

CRYSTALLINE AND PURE MODAFINIL AND PROCEDURES FOR ITS PRODUCTION

Crystals of bicalutamide and process for their production

Crystals of bicalutamide and process for their production

Process for purifying mesotrione

Organic-sulphide composition with masked odour

The present invention relates to the masking of the odour of organic sulphides and more particularly that of alkyl sulphides or of dialkyl sulphides, especially dimethyl sulphide, and also of oxides thereof, and especially of dimethyl sulphoxide, by addition to said organic sulphides of at least one odour-masking agent comprising at least one monoester, at least one diester or triester, at least one alcohol, at least one ketone and, optionally, at least one terpene.

Sulfur-containing compounds as solvents

Methods for using sulfur-containing compounds comprising short chain aliphatic ester or amide moieties as solvents and compositions comprising these compounds are provided.

CRYSTALS OF BICALUTAMIDE AND PROCESS FOR THEIR PRODUCTION

The invention relates to crystals of bicalutamide having a specific crystal form, and industrially practicable processes for the production of bicalutamide and crystals thereof which are excellent in environmental friendliness, economical efficiency, and safeness. The invention provides a process for the production of bicalutamide represented by formula (1): (1) characterized by comprising at least the step of reacting a compound represented by formula (3) with an oxidizing agent: (3) a process for the production of crystals of bicalutamide; and a crystal form of bicalutamide as determined by X-ray diffraction (XRD) or solid-state 13C NMR spectroscopy.

PRODUCTION PROCESS FOR MAGNESIUM N-ACETYL TAURINATE

The present invention concerns a process for the production of magnesium N-acetyl taurinate, in particular a process for the production of magnesium N-acetyltaurinate dihydrate.

PROCESS AND APPARATUS FOR MAKING ULTRA-PURE DMSO

One aspect of this invention relates to processes for solidifying dimethylsulfoxide including a step of partially solid-ifying a liquid phase including dimethylsulfoxide and one or more impurities, to form a mixture comprising solid dimethylsulfoxide and a liquid residue. In certain embodiments of the processes of the invention, ultra-high purity DMSO that exceeds the purity spec-ifications for U.S.P. grade DMSO can be produced by employing solidification, fractional solidification and/or melt crystallization processes.

CRYSTAL OF BICALUTAMIDE AND PRODUCTION METHOD THEREOF

The invention relates to crystals of bicalutamide having a specific crystal form, and industrially practicable processes for the production of bicalutamide and crystals thereof which are excellent in environmental friendliness, economical efficiency, and safeness. The invention provides a process for the production of bicalutamide represented by formula (1): (1) characterized by comprising at least the step of reacting a compound represented by formula (3) with an oxidizing agent: (3) a process for the production of crystals of bicalutamide; and a crystal form of bicalutamide as determined by X-ray diffraction (XRD) or solid-state 13C NMR spectroscopy.

CRYSTALLINE AND PURE MODAFINIL, AND PROCESS OF PREPARING THE SAME

The present invention provides an improved process for preparing modafinil, whereby it may be isolated in high purity by a single crystallization. The process produces modafinil free of sulphone products of over-oxidation and other byproducts. The invention further provides new crystalline Forms II-VI of modafinil and processes for preparing them. Each of the new forms is differentiated by a unique powder X-ray diffraction pattern. The invention further provides pharmaceutical compositions containing novel modafinil Forms II-IV and VI.

METHOD FOR THE MANUFACTURE OF POLY(ARYL ETHER KETONE)S IN THE PRESENCE OF SODIUM CARBONATE

The present invention relates to sodium carbonate (Na2CO3) having a certain particle size distribution and its use in preparing poly(aryl ether ketone)s, especially PEEK. Poly(aryl ether ketone)s made using the described sodium carbonate also make up a part of the invention. The present invention relates also to a method for providing a sodium carbonate having a certain particle size distribution, which is especially well suited for the preparation of poly(aryl ether ketone)s.

HIGH PURITY DIPHENYL SULFONE, PREPARATION AND USE THEREOF FOR THE PREPARATION OF A POLY(ARYLETHERKETONE)

The presence of certain impurities in diphenyl sulfone have a deleterious effect on the properties of the poly(aryletherketone)s produced therein, including one or more of color, melt stability, molecular weight, crystallinity, etc. and here identify those impurities and provide processes for the removal of such impurities.

CRYSTALLINE AND PURE MODAFINIL, AND PROCESS OF PREPARING THE SAME

The present invention provides an improved process for preparing modafinil, whereby it may be isolated in high purity by a single crystallization. The process produces modafinil free of sulphone products of over-oxidation and other byproducts. The invention further provides new crystalline Forms II-VI of modafinil and processes for preparing them. Each of the new forms is differentiated by a unique powder X-ray diffraction pattern. The invention further provides pharmaceutical compositions containing novel modafinil Forms II-IV and VI.

PURIFICATION OF HALOGENATED AROMATIC SULFONES OR KETONES

Abstract of the Disclosure A process for purifying a halogenated aromatic sulfone or ketone compound comprising contacting the compound with a solvent having a normal boiling point less than about 225°C to form a mixture, heating the mixture to a temperature above the normal boiling point of the solvent in a closed system to form a solution, cooling the solution to recrystallize the compound, and recovering the compound. A second embodiment of the invention comprises repeating the purification process steps at least once to further purify the halogenated aromatic sulfone or ketone compound.

COMPOSITION CONTAINING AT LEAST ONE AROMATIC BICYCLIC COMPOUND AND AT LEAST ONE 2-ALKYL ALCAN-1-OL OR AN ESTER, AND ITS USES

La présente invention concerne une composition renfermant au moins un composé bicyclique aromatique de formule générale (I) (voir formule I) ou un sel ou analogue chiral d'un tel composé, caractérisée en ce qu'elle comprend en outre au moins un 2-alkyl alcan-1-ol comprenant de 12 à 36 atomes de carbone, ou un ester d'un tel alcool. Le composé de formule (I) est de préférence l'acide 4-(3,5,5,8,8-pentaméthyl-5,6,7,8-tétrahydro-2-naphtylthio)benzoïque. L'invention concerne également les utilisations de cette composition, ainsi qu'un procédé de solubilisation du composé de formule (I) ci-dessus au moyen d'au moins un 2-alkyl alcan-1-ol.

The sulfur-containing compound as the solvent

Method for extracting garlic fructo-oligosaccharide

PROCESS FOR THE TREATMENT OF AN AQUEOUS MIXTURE COMPRISING A DIPOLAR APROTIC COMPOUND

CRYSTALLINE AND PURE MODAFINIL, AND PROCESS OF PREPARING THE SAME

IMPROVED PROCESS FOR PREPARING BENZHYDRYLTHIOACETAMIDE

The present invention is directed to an improved process for preparing modafinil wherein benzhydrylthioacetamide is prepared in high yield and purity by the reaction of a haloacetamide with the reaction product of thiourea and benzhydrol in aqueous solution. The reaction employing the haloacetamide is conducted in a solvent comprising water and an organic solvent such as dimethylformamide having dissolved therein a basic salt such as potassium carbonate. The resulting benzhydrylthioacetamide can be oxidized to provide the pharmaceutical modafinil.

NOVEL PROCESS

The present invention relates to a process for the preparation of polymorphic forms of the R- and S-enantiomers of modafinil, R-(-)-2-benzhydrylsulfinylacetamide and S-(+)-2- benzhydrylsulfinylacetamide respectively.

4-HYDROXY-4'-ISOPROPOXYDIPHENYL SULFONE DEVELOPER COMPOSITION, WET PULVERIZING METHOD, AND DISPERSION

A method of preventing hydration of 4-hydroxy-4'-isopropoxydiphenyl sulfone characterized by wet pulverizing the sulfone in water in the presence of a diphenyl sulfone derivative represented by general formula (I): (wherein R1 represents hydrogen or lower alkyl; R2 and R3 represent each independently lower alkyl; and n and m represent each an integer of 0, 1 to 4, provided when R1 is hydrogen, not both of m and n are 0 at the same time). A highly sensitive recording paper free from scumming can be produced by using a dispersion of a developer comprising the above sulfone.

Process for the preparation of armodafinil

The invention encompasses processes for preparing intermediates, such as R-modafinic acid or (R)-C_1-2 alkyl ester, of modafinic acid, and the conversion of the intermediates to armodafinil.

METHOD FOR PRODUCING MOLECULAR COMPOUND

PROCESS FOR THE PREPARATION OF AND CRYSTALLINE FORMS OF OPTICAL ENANTIOMERS OF MODAFINIL

The invention relates to a polymorphic form of (−)-modafinil that produces a powder X-ray diffraction spectrum comprising intensity peaks corresponding to interplanar spacings of about 14.14, 10.66, 7.80 and 4.02 Å, and a process for the preparation thereof. 1. A dextrorotatory enantiomer of modafinil in a polymorphic form that produces a powder X-ray diffraction spectrum comprising intensity peaks at the interplanar spacings: 8.54 , 4.27 , 4.02 , 3.98 (Å).2. The dextrorotatory enantiomer of modafinil according to claim 1 , wherein the polymorphic form produces a powder X-ray diffraction spectrum further comprising intensity peaks at the interplanar spacings: 13.40 claim 1 , 6.34 claim 1 , 5.01 claim 1 , 4.68 claim 1 , 4.62 claim 1 , 4.44 claim 1 , 4.20 claim 1 , 4.15 claim 1 , 3.90 claim 1 , 3.80 claim 1 , 3.43 (Å).3. A dextrorotatory enantiomer of modafinil in a polymorphic form that produces a powder X-ray diffraction spectrum comprising reflections at 15.4 claim 1 , 31.1 claim 1 , 33.1 and 33.4 degrees 2θ.4. The dextrorotatory enantiomer of modafinil according to claim 3 , wherein the polymorphic form produces a powder X-ray diffraction spectrum further comprising reflections at 9.8 claim 3 , 20.8 claim 3 , 26.4 claim 3 , 28.3 claim 3 , 28.7 claim 3 , 29.9 claim 3 , 31.6 claim 3 , 32 claim 3 , 34.1 claim 3 , 35.1 and 39 degrees 2θ.5. A pharmaceutical composition comprising a dextrorotatory enantiomer of modafinil according to .6. A pharmaceutical composition consisting essentially of a dextrorotatory enantiomer of modafinil according to .7. A Form I polymorph of (+)-modafinil.8. A pharmaceutical composition comprising a Form I polymorph of (+)-modafinil according to .9. A pharmaceutical composition consisting essentially of a Form I polymorph of (+)-modafinil according to .10. A process for preparing a Form I polymorph of (+)-modafinil comprising the steps of:(a) providing a solution of (+)-modafinil dissolved in a hot solvent;(b) rapidly cooling the solution ...

METHOD OF PURIFYING DIMETHYL SULFOXIDE

A method of purifying dimethyl sulfoxide economically and at good yield satisfies the specifications of the United States Pharmacopoeia and reduces odor. The method includes distilling a solution having 35 parts by weight or more of water admixed per 100 parts by weight of raw dimethyl sulfoxide. 17.-. (canceled)8. A method of purifying dimethyl sulfoxide comprising distilling a mixed solution prepared by adding 35 parts by weight or more of water to 100 parts by weight of raw dimethyl sulfoxide.9. The method as described in claim 8 , wherein the purified dimethyl sulfoxide has an absorbance of 0.01 to 0.20 at 275 nm.10. The method as described in claim 8 , wherein the water is ion-exchanged water claim 8 , distilled water claim 8 , ultrapure water claim 8 , or tap water.11. The method as described in claim 8 , wherein the water has an electrical conductivity of 50 mS/m or less at 25° C.12. The method as described in claim 8 , wherein the distillation is carried out in a single step to evaporate water to obtain dimethyl sulfoxide.13. The method as described in claim 8 , wherein the distillation is carried out in a first step to evaporate water to obtain roughly purified dimethyl sulfoxide claim 8 , followed by a second step of distilling the roughly purified dimethyl sulfoxide to obtain purified dimethyl sulfoxide.14. High-purity dimethyl sulfoxide obtained by a purification method as described in and having a purity of 99.996% or more as determined by gas chromatograph (GC) analysis.15. The method as described in claim 9 , wherein the water is ion-exchanged water claim 9 , distilled water claim 9 , ultrapure water claim 9 , or tap water.16. The method as described in claim 9 , wherein the water has an electrical conductivity of 50 mS/m or less at 25° C.17. The method as described in claim 10 , wherein the water has an electrical conductivity of 50 mS/m or less at 25° C.18. The method as described in claim 9 , wherein the distillation is carried out in a single step ...

PROCESS FOR PRODUCING 4,4`-DICHLORODIPHENYL SULFOXIDE

The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfoxide comprising: (I) reacting thionyl chloride, chlorobenzene and aluminum chloride in a molar ratio of thionyl chloride:chlorobenzene:aluminum chloride of 1:(6 to 9):(1 to 1.5) at a temperature in the range from 0 to below 20° C., forming an intermediate reaction product and hydrogen chloride; (II) mixing aqueous hydrochloric acid and the intermediate reaction product at a temperature in the range from 70 to 110° C. to obtain an organic phase comprising 4,4′-dichlorodiphenyl sulfoxide and an aqueous phase; (III) cooling the organic phase comprising the 4,4′-dichlorodiphenyl sulfoxide to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfoxide to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfoxide; (IV) solid-liquid-separation of the suspension to obtain a residual moisture containing solid 4,4′-dichlorodiphenyl sulfoxide comprising crystallized 4,4′-dichlorodiphenyl sulfoxide and mother liquor. 1. A process for producing 4 ,4′-dichlorodiphenyl sulfoxide comprising:(I) reacting thionyl chloride, chlorobenzene and aluminum chloride in a molar ratio of thionyl chloride:chlorobenzene:aluminum chloride of 1:(6 to 9):(1 to 1.5) at a temperature in the range from 0 to below 20° C., forming an intermediate reaction product and hydrogen chloride;(II) mixing aqueous hydrochloric acid and the intermediate reaction product at a temperature in the range from 70 to 110° C. to obtain an organic phase comprising 4,4′-dichlorodiphenyl sulfoxide and an aqueous phase;(III) cooling the organic phase comprising the 4,4′-dichlorodiphenyl sulfoxide to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfoxide to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfoxide, wherein cooling of the organic phase is carried out in a gastight closed vessel by(i) reducing the pressure in the gastight closed vessel;(ii) evaporating solvent;(iii) ...

PROCESS FOR PRODUCING 4,4'-DICHLORODIPHENYL SULFOXIDE

The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfoxide comprising: (a) reacting thionyl chloride, chlorobenzene and aluminum chloride in a molar ratio of thionyl chloride:chlorobenzene:aluminum chloride of 1:(6 to 9):(1 to 1.5) at a temperature in the range from 0 to below 20° C., forming an intermediate reaction product and hydrogen chloride, (b) mixing aqueous hydrochloric acid and the intermediate reaction product at a temperature in the range from 70 to 110° C. to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfoxide, (c) separating the crude reaction product into an organic phase comprising the 4,4′-dichlorodiphenyl sulfoxide and an aqueous phase, (d) washing the organic phase with an extraction liquid.

A PROCESS FOR OBTAINING 4,4'-DICHLORODIPHENYL SULFOXIDE

The invention relates to a process for obtaining 4,4′-dichlorodiphenyl sulfoxide from a liquid mixture comprising dichlorodiphenyl sulfoxide and a solvent, comprising: (a) cooling the liquid mixture to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfoxide in the solvent to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfoxide, (b) solid-liquid-separation of the suspension to obtain a residual moisture containing solid 4,4′-dichlorodiphenyl sulfoxide as a product and mother liquor, (c) concentrating the mother liquor, (d) recycling at least a part of the concentrated mother liquor into the cooling step (a).

PROCESS FOR PURIFYING 4,4'-DICHLORODIPHENYL SULFOXIDE

The invention relates to a process for purifying 4,4′-dichlorodiphenyl sulfoxide comprising: (a) providing a suspension comprising particulate 4,4′-dichlorodiphenyl sulfoxide in monochlorobenzene, (b) solid-liquid separation of the suspension to obtain residual moisture containing 4,4′-dichlorodiphenyl sulfoxide, (c) washing residual moisture containing 4,4′-dichlorodiphenyl sulfoxide with monochlorobenzene, (d) optionally repeating steps (a) to (c).

GLUCAGON RECEPTOR ANTAGONISTS

Provided herein are solid state forms of compounds, including enantiomerically pure forms thereof, and pharmaceutically acceptable salts or co-crystals and prodrugs thereof which have glucagon receptor antagonist or inverse agonist activity. Further, provided herein are pharmaceutical compositions and methods of treating, preventing, ameliorating, delaying the time to onset or reducing the risk for the development or progression of at least one condition, disease, or disorder for which one or more glucagon receptor antagonist is indicated, including Type I and II diabetes, insulin resistance, hyperglycemia, ketoacidosis, or ketosis. 1. A crystalline form selected from the group consisting of a crystalline form of sodium (R)-2-(4-(2-(4′-(tert-butyl)-[1 ,1′-biphenyl]-4-yl)-3-oxo-3-((2′ ,4′ ,6′-trimethyl-[1 ,1′-biphenyl]-4-yl)amino)propyl)benzamido)ethane-1-sulfonate characterized as Form A , a crystalline form of calcium (R)-2-(4-(2-(4′-(tert-butyl)-[1 ,1′-biphenyl]-4-yl)-3-oxo-3-((2′ ,4′ ,6′-trimethyl-[1 ,1′-biphenyl]-4-yl)amino)propyl)benzamido)ethane-1-sulfonate characterized as Form B , and a crystalline form of potassium (R)-2-(4-(2-(4′-(tert-butyl)-[1 ,1′-biphenyl]-4-yl)-3-oxo-3-((2′ ,4′ ,6′-trimethyl-[1 ,1′-biphenyl]-4-yl)amino)propyl)benzamido)ethane-1-sulfonate characterized as Form C.2. Form A of claim 1 , wherein Form A is characterized by one or more peaks in an X-ray powder diffraction pattern claim 1 , wherein the one or more peaks is selected from the group consisting of a peak from about 4.2 to about 4.8 degrees claim 1 , a peak from about 6.7 to about 7.1 degrees claim 1 , a peak from about 9.0 to about 9.4 degrees claim 1 , a peak from about 10.8 to about 11.2 degrees claim 1 , a peak from about 11.1 to about 11.5 degrees claim 1 , a peak from about 11.7 to about 12.1 degrees claim 1 , a peak from about 13.5 to about 13.9 degrees claim 1 , a peak from about 21.2 to about 21.6 degrees claim 1 , and a peak from about 23.6 to about 24.0 degrees claim 1 ...

PROCESS FOR THE OXIDATION OF SULFOXIDES

The present invention relates to a process for oxidizing a sulfoxide to the respective sulfone, said process comprising reacting the sulfoxide with hydrogen peroxide in the presence of a catalyst, obtaining a mixture (M) comprising the sulfone and the catalyst, wherein the catalyst comprises a porous titanium-containing silicate as a catalytically active material. 1. A process for oxidizing a sulfoxide to a sulfone , said process comprising(i) reacting the sulfoxide with hydrogen peroxide in the presence of a catalyst, obtaining a mixture (M) comprising the sulfone and the catalyst,wherein the catalyst comprises a porous titanium-containing silicate as a catalytically active material.3. The process of claim 1 , wherein the sulfoxide is 4 claim 1 ,4′-dichlorodiphenylsulfoxide or 4 claim 1 ,4′-dihydroxydiphenylsulfoxide.4. The process of claim 1 , wherein the porous titanium-containing silicate comprised in the catalyst is a titanium-containing zeolitic material having a zeolitic framework structure comprising titanium and silicon.5. The process of claim 4 , wherein the framework structure of the titanium-containing zeolitic material comprised in the catalyst is an MWW-type framework structure.6. The process of claim 5 , wherein the framework structure of the titanium-containing zeolitic material comprised in the catalyst has a titanium content in a range of from 0.5 to 3.0 weight-% claim 5 , calculated as element and based on a total weight of the titanium-containing zeolitic material claim 5 , and a silicon content in a range of from 30 to 50 weight-% claim 5 , calculated as element and based on the total weight of the titanium-containing zeolitic material.7. The process of claim 1 , wherein the hydrogen peroxide used in (i) is employed as an aqueous hydrogen peroxide solution claim 1 , having a hydrogen peroxide content in a range of from 10 to 70 weight-% claim 1 , based on a total weight of the aqueous solution.8. The process of claim 1 , wherein at the beginning ...

DMSO PURIFICATION

Methods and apparatus for purifying DMSO are disclosed including a method of purifying DMSO involving providing a first DMSO composition having impurities; freezing a portion of the first DMSO composition on a first surface to form a second DMSO composition having higher DMSO purity than the first DMSO composition such that a third DMSO composition remains from the unfrozen portion of the first DMSO composition; separating the second DMSO composition from the third DMSO composition; and melting a portion of the second DMSO composition. The freezing of the portion of the first DMSO composition, the separating of the second DMSO composition from the third DMSO composition, and the melting of the portion of the second DMSO composition may happen simultaneously. DMSO purification apparatus employing such methods and other methods are also taught. 1. a DMSO purification apparatus comprising:a. a first surface;b. a second surface;c. a DMSO supply;d. a purified DMSO discharge;e. wherein the first surface is a first heat conducting surface;f. wherein the second surface is a second heat conducting surface;g. wherein the first surface is arranged and configured to freeze DMSO; andh. wherein the second surface is arranged and configured to melt DMSO at the same time the first surface freezes DMSO.2. The DMSO purification apparatus of wherein the first surface is a part of a chilled drum.3. The DMSO purification apparatus of further comprising a vessel containing a volume of DMSO.4. The DMSO purification apparatus of wherein the volume of DMSO is adjacent to the first surface.5. The DMSO purification apparatus of wherein the volume of DMSO is mixed.6. The DMSO purification apparatus of wherein the chilled drum is arranged and configured to rotate through a volume of liquid DMSO thereby freezing a portion of the volume of liquid DMSO to the chilled drum.7. The DMSO purification apparatus of further comprising a mechanical separator arranged and configured to direct a quantity of ...

Process for producing 4,4'-dichlorodiphenyl sulfone

The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone, comprising: (I) reacting thionyl chloride, chlorobenzene and aluminum chloride forming an intermediate reaction product and hydrogen chloride; (II) mixing aqueous hydrochloric acid and the intermediate reaction product to obtain an organic phase comprising 4,4′-dichlorodiphenyl sulfoxide and an aqueous phase; (III) cooling the organic phase to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfoxide to obtain a suspension; (IV) solid-liquid-separation of the suspension to obtain crystallized 4,4′-dichlorodiphenyl sulfoxide, and mother liquor; (V) washing the crystallized 4,4′-dichlorodiphenyl sulfoxide with a carboxylic acid to obtain carboxylic acid-wet 4,4′-dichlorodiphenyl sulfoxide; (VI) reacting the washed 4,4′-dichlorodiphenyl sulfoxide and an oxidizing agent in a carboxylic acid as solvent to obtain a reaction mixture comprising 4,4′-dichlorodiphenyl sulfone and carboxylic acid; (VII) separating the reaction mixture comprising 4,4′-dichlorodiphenyl sulfone and carboxylic acid into a residual moisture comprising 4,4′-dichlorodiphenyl sulfone as crude product and a liquid phase comprising carboxylic acid.

METHOD FOR PURIFYING SULFONATED AROMATIC MONOMER

The present invention relates to an improved method for purifying a sulfonated aromatic monomer. The method is an economical method capable of providing a highly pure sulfonated aromatic monomer, in which a salt precipitation step and a recrystallization step are simplified while maintaining the reaction conditions used in a conventional method for synthesizing the sulfonated aromatic monomer, and a purification process is carried out using an easily available and stable chemical substance. The sulfonated aromatic monomer obtained by the purification method will be useful for the preparation of a polymer for a polymer electrolyte membrane and will be advantageous to synthesize polymer with high molecular weight. 2. The method of claim 1 , wherein the step of adding the salt to precipitate the crude compound is performed by adding the salt to the compound 2 placed on ice.3. The method of claim 1 , wherein the step of dissolving the crude compound is carried out after washing the crude compound with alcohol selected from among methanol claim 1 , ethanol or a mixture thereof.4. The method of claim 1 , wherein the step of neutralizing the aqueous solution containing the crude compound is carried out using any one weak base selected from the group consisting of sodium carbonate claim 1 , sodium hydrogen carbonate claim 1 , ammonium hydroxide claim 1 , ammonia claim 1 , sodium phosphate and sodium sulfate.5. The method of claim 1 , wherein the step of neutralizing the aqueous solution containing the crude compound is carried out by neutralizing the aqueous solution with anion exchange resin claim 1 , followed by a washing step.6. The method of claim 5 , wherein the washing step is carried out by washing the anion exchange resin with the same amount of a base as that of the anion exchange resin. The present invention relates to an improved method for purifying a sulfonated aromatic monomer, and more particularly to an economical method for purifying a sulfonated aromatic ...

A PROCESS FOR OBTAINING 4,4'-DICHLORODIPHENYL SULFONE

The invention relates to a process for obtaining 4,4′-dichlorodiphenyl sulfone from an organic mixture comprising 4,4′-dichlorodiphenyl sulfone and a linear Cto Ccarboxylic acid as organic solvent, comprising: (a) cooling the organic mixture by (a1a) mixing the organic mixture with water in a crystallization vessel to obtain a liquid mixture; (a1b) cooling the liquid mixture obtained in (a1a) to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfone by (i) reducing the pressure in the crystallization vessel to a pressure at which the water starts to evaporate, (ii) condensing the evaporated water by cooling, (iii) mixing the condensed water into the liquid mixture in the crystallization vessel, to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfone; or by (a2) bringing the organic mixture into contact with at least one coolable surface and thereby reducing the temperature in the organic mixture with a cooling rate in the range from 5 to 50 K/h until a temperature in the range from 10 to 30° C. is reached, wherein the organic mixture and the at least one coolable surface have a temperature difference which is kept during the whole cooling process in the range from 1 to 30 K to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfone. (b) carrying out a solid-liquid-separation of the suspension obtained in (a1b) or in (a2) to obtain a residual moisture containing solid 4,4′-dichlorodiphenyl sulfone as product and mother liquor comprising the organic solvent and water. 116.-. (canceled)17. A process for obtaining 4 ,4′-dichlorodiphenyl sulfone from an organic mixture comprising 4 ,4′-dichlorodiphenyl sulfone and a linear Cto Ccarboxylic acid as organic solvent , comprising: (a1a) mixing the organic mixture with water in a crystallization vessel to obtain a liquid mixture;', (i) reducing the pressure in the crystallization vessel to a pressure at which the water starts to evaporate,', '(ii) condensing the ...

HIGH PURITY DIPHENYL SULFONE, PREPARATION AND USE THEREOF FOR THE PREPARATION OF A POLY(ARYLETHERKETONE)

The presence of certain impurities in diphenyl sulfone have a deleterious effect on the properties of the poly(aryletherketone)s produced therein, including one or more of color, melt stability, molecular weight, crystallinity, etc. and here identify those impurities and provide processes for the recovery of the diphenyl sulfone. 2. The method according to claim 1 , wherein said used DPS further comprises therein more than 0.03 area % of one or more oligo(aryl ether ketone) impurities claim 1 , wherein area % represents the ratio of the LC peak area of the impurity of concern over the total area of all LC peaks of the used DPS.4. The method according to wherein said used DPS comprises at least one fluorinated monomer.6. The method according to claim 1 , wherein said used DPS further meets the following impurity limitation:a water content of less than 0.1 wt. %.7. The method according to claim 1 , wherein the poly(aryletherketone) is poly(ether ether ketone).8. The method according to claim 1 , wherein said used DPS is purified by distillation claim 1 , liquid chromatography claim 1 , adsorption and/or absorption on silica or other solid media claim 1 , ion exchange techniques claim 1 , extraction claim 1 , (re)crystallization and/or precipitation.9. The method according to claim 1 , which is a method by aromatic nucleophilic substitution in the presence of particulate sodium carbonate claim 1 , wherein said particulate sodium carbonate has a particle size distribution as follows:{'sub': 90', '90', '99.5, 'D≧45 μm and D≦250 μm and D≦710 μm.'}10. The method according to claim 1 , which is a method for the preparation of a semi-crystalline poly(aryl ether ketone) by aromatic nucleophilic substitution claim 1 , wherein a nucleophile is reacted with a 4 claim 1 ,4′-difluorobenzophenone claim 1 , said 4 claim 1 ,4′-difluorobenzophenone meeting the following impurity limitation:[2,4′-difluorobenzophenone]+[4-monofluorobenzophenone]≦1250 ppm,wherein the amounts of 2,4′- ...

METHOD FOR RECOVERING DIMETHYL SULFOXIDE FROM RECOVERED RESIST REMOVER

A method for recovering dimethyl sulfoxide, including a step of contacting a recovered resist remover containing at least one compound selected from the group consisting of glycol ether, glycol and triol, and dimethyl sulfoxide with water and performing distillation. 1. A method for recovering dimethyl sulfoxide , comprising a step of contacting a recovered resist remover containing at least one compound selected from the group consisting of glycol ether , glycol and triol , and dimethyl sulfoxide with water and performing distillation.2. The recovering method according to claim 1 , wherein the compound is at least one selected from the group consisting of 3-methoxy-3-methyl-1-butanol claim 1 , diethylene glycol claim 1 , propylene glycol claim 1 , glycerin and 2-(2-methoxyethoxy)ethanol.3. The recovering method according to claim 1 , wherein the compound is 3-methoxy-3-methyl-1-butanol. The present invention relates to a method for recovering dimethyl sulfoxide (DMSO) from a recovered resist remover.When a semiconductor element or the like is manufactured by photolithography, after a fine circuit or the like is formed by etching, an unnecessary resist film or an etching residue is washed and removed by using a resist remover. As the resist remover, an aqueous solution of sodium hydroxide or a general organic solvent can be used alone, but the peelability is not sufficient, and a variety of resist removers have been proposed so far in order to improve the peelability.As a resist remover having high peelability, for example, a solution obtained by dissolving a quaternary ammonium hydroxide such as tetramethylammonium hydroxide (TMAH) in a mixed solvent of DMSO and glycol ether such as 3-methoxy-3-methyl-1-butanol (MMB) is often used (PTL 1).PTL 1: WO 2010/073430 A1Currently, used resist removers (recovered resist removers) are usually discarded as industrial waste. On the other hand, DMSO used in the resist remover as described above is also used as a rinse liquid in ...

A PROCESS FOR PRODUCING 4,4'-DICHLORODIPHENYL SULFONE

The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone, comprising: (a) reacting 4,4′-dichlorodiphenyl sulfoxide and an oxidizing agent in at least one carboxylic acid as solvent to obtain a reaction mixture comprising 4,4′-dichlorodiphenyl sulfone and carboxylic acid; (b) separating the reaction mixture into a first stream comprising 4,4′-dichlorodiphenyl sulfone and a second stream comprising carboxylic acid; (c) purifying the second stream comprising carboxylic acid by distilling a part of the second stream comprising carboxylic acid stripping low boilers from at least a part of the second stream comprising carboxylic acid (d) recycling the purified carboxylic acid into the reaction (a). 118.-. (canceled)19. A process for producing 4 ,4′-dichlorodiphenyl sulfone , comprising:(a) reacting 4,4′-dichlorodiphenyl sulfoxide and an oxidizing agent in at least one carboxylic acid as solvent to obtain a reaction mixture comprising 4,4′-dichlorodiphenyl sulfone and the at least one carboxylic acid;(b) separating the reaction mixture into a first stream comprising 4,4′-dichlorodiphenyl sulfone and a second stream comprising the at least one carboxylic acid;(c) purifying the second stream comprising the at least one carboxylic acid bydistilling a part of the second stream comprising the at least one carboxylic acid;stripping low boilers from at least a part of the second stream comprising the at least one carboxylic acid;(d) recycling the purified at least one carboxylic acid into the reaction (a).20. The process according to claim 19 , wherein purifying the second stream comprising the at least one carboxylic acid comprises:(a1) stripping low boilers from the second stream comprising the at least one carboxylic acid in a stripping column using a stripping gas to obtain a crude carboxylic acid;(b1) separating the crude carboxylic acid into a first carboxylic acid stream and a second carboxylic acid stream;(c1) distilling the second carboxylic acid ...

PROCESS FOR THE PRODUCTION OF ALKANESULFONIC ACIDS

The present invention deals with a process for the production of alkanesulfonic acids, in particular methanesulfonic acid, and a method of purification of the raw products. 1. A process for preparing an alkanesulfonic acid , the process comprising:reacting sulfur trioxide and an alkane to obtain a raw alkane sulfonic acid; andpurifying the raw alkane sulfonic acid in a distillation process comprising at least two steps, to obtain a purified alkanesulfonic acid.2. The process according to claim 1 , wherein the distillation process employs a distillation set-up comprising (i) one distillation column with high separation performance (main distillation) claim 1 , and (ii) at least one additional distillation column claim 1 , either before and/or after the main distillation column claim 1 , each with a separation performance not matching that of the main distillation column (pre-distillation and/or post-distillation claim 1 , respectively).3. The process according to claim 1 , wherein the alkanesulfonic acid is methanesulfonic acid (MSA) and the alkane is methane.4. The process according to claim 1 , wherein the distillation process is operated at a temperature in the range of 130° C. to 200° C. in all distillation columns.5. The process according to claim 1 , wherein the distillation process is operated at a pressure in the range of 0.1 to 30 mbar in all distillation columns.6. The process according to claim 1 , wherein the distillation process is performed in at least two separate distillation columns.7. The process according to claim 1 , wherein the distillation process consists of two or three separate distillation columns.8. The process according to claim 1 , wherein the distillation process occurs such that each distillation step is carried out in one column or in more than one column operated in parallel.9. The process according to claim 1 , wherein a first distillation step claim 1 , a third distillation step claim 1 , or both is performed in a reaction vessel ...

METHOD FOR SEPARATION OF METHIONINE SULFOXIDE DIASTEREOMERS

A method of separating a compound having methionine oxide diastereomers, including: loading a diastereomeric mixture into a chromatography column, the diastereomeric mixture of a compound having a plurality of methionine oxide diastereoisomers. The method also includes passing a mobile phase, the mobile phase including a supercritical fluid, through the chromatography column to separate the compound based on each methionine oxide diastereoisomer of the plurality of methionine oxide diastereoisomers in the chromatography column. 1. A method for producing a diasteriomerically pure methionine sulfoxide composition , the method comprising:loading a diastereomeric mixture of compositions that contain at least one of S-methionine sulfoxide (Met-(S)-SO) or R-methionine sulfoxide (Met-(R)-SO) onto a chromatography column; andpassing a mobile phase, the mobile phase including a supercritical fluid, through the chromatography column to separate compositions that contain Met-(S)-SO from those that contain Met-(R)-SO using the chromatography column, thereby producing a diastereomerically pure methionine sulfoxide composition.2. The method according to claim 1 , further comprising:dissolving the diastereomeric mixture in an eluent.3. The method according to claim 2 , wherein the eluent is ethanol.4. The method according to claim 1 , wherein the supercritical fluid is selected from the group consisting of carbon dioxide claim 1 , nitrous oxide claim 1 , ammonia claim 1 , and combinations thereof.5. The method according to claim 1 , wherein the supercritical fluid is present from about 50% to about 60% of the mobile phase.6. The method according to claim 1 , wherein the mobile phase further includes a co-solvent.7. The method according to claim 6 , wherein the co-solvent is selected from the group consisting of methanol claim 6 , isopropanol claim 6 , methylene chloride claim 6 , tetrahydrofuran claim 6 , acetonitrile claim 6 , and combinations thereof.8. The method according to ...

METHODS AND DEVICES TO GENERATE [F-18]TRIFLYL FLUORIDE AND OTHER [F-18] SULFONYL FLUORIDES

Described herein are methods and devices that allow the generation of [F-18]triflyl fluoride and other [F-18] sulfonyl fluorides (such as [F-18]tosyl fluoride) in a manner that is suitable for radiosynthesis of F-18 labeled radiopharmaceuticals using currently available synthesis modules. 1. A method of making [F-18]sulfonyl fluoride without any evaporation step , the method comprising:a) passing an aqueous [F-18]fluoride solution or solvent through a solid phase extraction column comprising an anion-exchange resin so that the [F-18]fluoride is trapped on the resin;b) rinsing the resin with an organic solvent to eliminate residual water; and{'sub': 2', '2, 'sup': '1', 'c) eluting the [F-18]fluoride with an eluting solution to release the [F-18]fluoride from the anion-exchange resin as [F-18]RSOF which acts as a source of [F-18]fluoride for a labeling reaction, wherein the eluting solution comprises a compound having the formula RSORand an organic solvent, wherein'}R is selected from the group consisting of hydrocarbyl, substituted hydrocarbyl, alkyl, substituted alkyl, cycloalkyl, substituted cycloalkyl, alkenyl, substituted alkenyl, alkynyl, substituted alkynyl, aryl, substituted aryl, alkylaryl, substituted alkylaryl, arylalkyl, substituted arylalkyl, arylalkenyl, substituted arylalkenyl, arylalkynyl, substituted arylalkynyl, heteroaryl, substituted heteroaryl, methyl, trifluoromethyl, and combinations thereof;{'sup': '1', 'Ris a leaving group; and'}wherein all method steps are performed with a single peristaltic pump.2. The method of claim 1 , wherein the eluting is done via a circulating method with the single peristaltic pump.3. The method of claim 1 , wherein the single peristaltic pump provides air flow to separate [F-18]sulfonyl fluoride from the reaction mixture.4. The method of claim 3 , wherein a separator is used to separate [F-18]triflyl fluoride from the reaction mixture using the air flow provided by the pump5. The method of claim 4 , wherein the ...

Process for preparing an organic sulfone

A process for preparing polyaryl ethers in which a polycondensation of the monomer building blocks is carried out using microwave irradiation leads to thermoplastic molding compositions having improved color properties.

Process for preparing 3-methylsulfonylpropionitrile

The present invention relates to processes for preparing 3-methylsulfonylpropionitrile. The processes provide a good yield and a good purity of the final product and provide a controllable reaction. The present invention also relates to a crystalline form of 3-methylsulfonylpropionitrile having X-ray diffraction peaks at 13.9±0.1, 19.2±0.1, 20.0±0.1, 22.5±0.1, 23.2±0.1, 25.7±0.1, 28.1±0.1, 29.9±0.1, and 30.6±0.1 degrees 20, and wherein the most intense peak is the peak at 13.9±0.1 degrees 20.

Method for refining 2-nito-4-methylsulfonyl benzoic acid and intermediate thereof

A method for refining a 2-nitro-4-methylsulfonyl benzoic acid and an intermediate thereof are provided, wherein the method includes steps of: using a crude 2-nitro-4-methylsulfonyl benzoic acid (I) as a raw material; using organic amine (II) as a base; synthesizing an intermediate, which is an amine salt (III), in an organic solvent; treating the amine salt (III) with an inorganic base in an aqueous phase to obtain an inorganic metal salt (IV) or an inorganic metal salt (IV′); and acidifying by adding an inorganic acid to obtain a fine 2-nitro-4-methylsulfonyl benzoic acid (I).

Process for the Synthesis of Chiral Propargylic Alcohols

A process for the synthesis of chiral propargylic alcohols. 113-. (canceled)15. The process of claim 14 , wherein the protic chiral auxiliary is selected from the group consisting of N claim 14 ,N-disubstituted ephedrine derivatives.16. The process of claim 14 , wherein the molar ratio of the protic chiral auxiliary to the diorganylzinc(II) compound is in the range of 1.5:1 to 1:1.17. The process of claim 14 , wherein the diorganylzinc(II) compound is selected from the group consisting of di(C-alkyl) and di(C-cycloalkyl) claim 14 , wherein the alkyl moieties are selected from the group consisting of methyl claim 14 , ethyl claim 14 , propyl claim 14 , isopropyl claim 14 , butyl claim 14 , isobutyl claim 14 , sec-butyl and tert-butyl claim 14 , pentyl claim 14 , hexyl claim 14 , heptyl claim 14 , and octyl claim 14 , and wherein the cycloalkyl moieties are selected from the group consisting of cyclopropyl claim 14 , cyclobutyl claim 14 , cyclopentyl and cyclohexyl.18. The process of claim 14 , wherein in step (i) the molar ratio of the protic chiral auxiliary to the compound of formula III is in the range of 1:1 to 1:10 claim 14 , preferably in the range of 1:2 to 1:6 claim 14 , more preferably of 1:3 to 1:6.19. The process of claim 14 , wherein in step (iii) the compound of formula II is used in a molar ratio to the compound of formula III of 1:0.6 to 1:1.3.201. The process of claim claim 14 , wherein the organolithium base and/or the other alkali metal organyl is added in a molar ratio to the compound of formula III from 1:0.8 to 1:1.5.21. The process of claim 14 , wherein the organolithium base is selected from the group consisting of (C-alkyl)lithium claim 14 , lithium diisopropylamide (LDA) claim 14 , lithium hexamethyldisilazide (LiHMDS) claim 14 , phenyllithium claim 14 , and naphthyllithium.22. The process of claim 21 , wherein the (C-alkyl)lithium is selected from the group consisting of methyllithium claim 21 , n-butyllithium claim 21 , sec-butyllithium ...

METHOD OF DISTILLING DIMETHYL SULFOXIDE AND MULTISTAGE DISTILLATION TOWER

A method of distilling a liquid containing dimethyl sulfoxide using a distillation system, including mixing sodium carbonate with a liquid containing dimethyl sulfoxide at a bottom of the distillation system such that sodium carbonate accounts for 0.005% to 25% by weight relative to 100% by weight of the liquid containing dimethyl sulfoxide and sodium carbonate in total at the bottom of the distillation system and heating the bottom; and obtaining a distillate containing dimethyl sulfoxide at a position lower than a position at which the liquid containing dimethyl sulfoxide is introduced and higher than a position of the heating portion. 115.-. (canceled)16. A method of distilling a liquid containing dimethyl sulfoxide using a distillation system , comprising:(1) mixing sodium carbonate with a liquid containing dimethyl sulfoxide at a bottom of the distillation system such that sodium carbonate accounts for 0.005% to 25% by weight relative to 100% by weight of the liquid containing dimethyl sulfoxide and sodium carbonate in total at the bottom of the distillation system and heating the bottom; and(2) obtaining a distillate containing dimethyl sulfoxide at a position lower than a position at which the liquid containing dimethyl sulfoxide is introduced and higher than a position of the heating portion.17. The method according to claim 16 , wherein a distillate rich in dimethyl sulfoxide compared to a feed material supplied to the distillation equipment is obtained at the position lower than the position at which the liquid containing dimethyl sulfoxide is initially introduced and higher than the position of the heated portion.18. The method according to claim 16 , wherein the distillation system is a single multistage distillation tower.19. The method according to claim 16 , wherein the temperature of the bottom of the distillation system is 90° C. to 180° C.20. The method according to claim 16 , wherein sodium carbonate is directly added at the bottom of the ...

HIGH PURITY DIPHENYL SULFONE, PREPARATION AND USE THEREOF FOR THE PREPARATION OF A POLY(ARYLETHERKETONE)

The presence of certain impurities in diphenyl sulfone have a deleterious effect on the properties of the poly(aryletherketone)s produced therein, including one or more of color, melt stability, molecular weight, crystallinity, etc. and here identify those impurities and provide processes for the recovery of the diphenyl sulfone. 1. A method for the recovery of a diphenyl sulfone that has been used in the preparation of a poly(aryletherketone) comprising isolating diphenyl sulfone from a diphenyl sulfone mixture [herein after DPS solution] comprising at least one of the following: at least one low boiling organic solvent , water , one or more inorganic salts like chlorides , fluorides and carbonates , residual monomer(s) , and residual oligo(aryl ether ketone)s.2. The method according to claim 1 , characterized in that the diphenyl sulfone solubility in said DPS solution is lowered at a level of at or below 1.5 wt. % by a step selected from the group consisting of:a) addition of a non solvent to the solution;b) addition of the solution to a non solvent;c) removal of a fraction of low boiling organic solvent present in the solution by a low temperature evaporation process, followed or preceded by addition of a non solvent to the solution;d) cooling the solution; ande) any combination of two or more steps a), b), c) and d).3. The method according to claim 2 , wherein the non-solvent is selected from a group consisting of water claim 2 , methanol claim 2 , ethanol and mixtures thereof.4. The method according to claim 2 , wherein the low temperature evaporation process of c) is carried out in wiped-film evaporator operating under vacuum. The present application is a divisional filed pursuant to 35 U.S.C. §121 of U.S. patent application Ser. No. 14/246,901 filed on Apr. 7, 2014 which is a continuation of U.S. patent application Ser. No. 13/125,508 filed on Apr. 21, 2011, now U.S. Pat. No. 8,710,171 which claims the priority benefit to U.S. provisional application No. 61/ ...

Process for preparation of apremilast and its intermediates

Present application relates to the process for the preparation of 1-(3-Ethoxy-4-methoxy-phenyl)-2-methanesulf-onyl-ethylamine of the formula (II), its resolution and its use in preparation of Apremilast of formula (I), process for the preparation of crystalline form B of apremilast, process for preparation of amorphous form of apremilast and the crystalline form of (S)-1-(3-Eth-oxy-4-methoxy-phenyl)-2-methanesulfonyl-ethylamine of the formula (Va).

Process for preparing mesotrione

A process for the preparation of mesotrione enolate is provided. The process comprises providing a solution of mesotrione in an organic solvent and contacting the solution with a moderate base in the presence of water at a pH of from 6 to 8, to form an aqueous mesotrione enolate solution. A process for preparing mesotrione from the products of an enol ester rearrangement of 3-oxocyclohex-1-enyl-4-(methylsulfonyl)-2-nitrobenzoate is also provided. The process comprises contacting the products of the rearrangement reaction with an organic solvent to dissolve mesotrione; and contacting the resulting solution with an aqueous solution of an acid.

METHOD OF PURIFYING DIMETHYL SULFOXIDE

A method of purifying dimethyl sulfoxide includes distilling a dimethyl sulfoxide-containing liquid in the presence of sodium carbonate under a reduced pressure in an inert gas atmosphere to distill out dimethyl sulfoxide, an amount of the sodium carbonate with respect to 100 g of pure dimethyl sulfoxide in a residual liquid after the distillation being 6 times or more the amount of the sodium carbonate with respect to 100 g of the pure dimethyl sulfoxide in the dimethyl sulfoxide-containing liquid before the distillation. 1. A method of purifying dimethyl sulfoxide comprising distilling a dimethyl sulfoxide-containing liquid in the presence of sodium carbonate under reduced pressure in an inert gas atmosphere to distill out dimethyl sulfoxide , an amount of the sodium carbonate with respect to 100 g of pure dimethyl sulfoxide in a residual liquid after the distillation being 6 times or more the amount of the sodium carbonate with respect to 100 g of the pure dimethyl sulfoxide in the dimethyl sulfoxide-containing liquid before the distillation.2. The method according to claim 1 , wherein the distillation is performed by adding claim 1 , at a start of the distillation claim 1 , the sodium carbonate in an amount of 0.0005 to 1.0 g with respect to 100 g of the pure dimethyl sulfoxide in the dimethyl sulfoxide-containing liquid.3. The method according to claim 1 , wherein the amount of the sodium carbonate with respect to 100 g of the pure dimethyl sulfoxide in the residual liquid after the distillation is 6 to 1000 times the amount of the sodium carbonate with respect to 100 g of the pure dimethyl sulfoxide in the dimethyl sulfoxide-containing liquid before the distillation.4. The method according to claim 1 , wherein the amount of the sodium carbonate in the residual liquid after the distillation is 0.01 to 100 g with respect to 100 g of the pure dimethyl sulfoxide in the residual liquid after the distillation.5. The method according to claim 1 , wherein claim 1 , ...

METHOD OF PURIFYING DIMETHYL SULFOXIDE

A method of purifying dimethyl sulfoxide includes distilling a dimethyl sulfoxide-containing liquid in the presence of sodium carbonate in an inert gas atmosphere to distill out dimethyl sulfoxide, an amount of the sodium carbonate with respect to 100 g of pure dimethyl sulfoxide in a residual liquid after the distillation being 6 times or more the amount of the sodium carbonate with respect to 100 g of the pure dimethyl sulfoxide in the dimethyl sulfoxide-containing liquid before the distillation. 17-. (canceled)8. A method of purifying dimethyl sulfoxide comprising distilling a dimethyl sulfoxide-containing liquid in the presence of sodium carbonate in an inert gas atmosphere to distill out dimethyl sulfoxide , an amount of the sodium carbonate with respect to 100 g of pure dimethyl sulfoxide in a residual liquid after the distillation being 6 times or more the amount of the sodium carbonate with respect to 100 g of the pure dimethyl sulfoxide in the dimethyl sulfoxide-containing liquid before the distillation.9. The method according to claim 8 , wherein the distillation is performed by adding claim 8 , at a start of the distillation claim 8 , the sodium carbonate in an amount of 0.0005 to 1.0 g with respect to 100 g of the pure dimethyl sulfoxide in the dimethyl sulfoxide-containing liquid.10. The method according to claim 8 , wherein the amount of the sodium carbonate with respect to 100 g of the pure dimethyl sulfoxide in the residual liquid after the distillation is 6 to 1000 times the amount of the sodium carbonate with respect to 100 g of the pure dimethyl sulfoxide in the dimethyl sulfoxide-containing liquid before the distillation.11. The method according to claim 8 , wherein the amount of the sodium carbonate in the residual liquid after the distillation is 0.01 to 100 g with respect to 100 g of the pure dimethyl sulfoxide in the residual liquid after the distillation.12. The method according to claim 8 , wherein claim 8 , after water in the dimethyl ...

Production process for magnesium N-acetyl taurinate

The present invention concerns a process for the production of magnesium N-acetyl taurinate, in particular a process for the production of magnesium N-acetyltaurinate dihydrate. 1. Production process for magnesium N-acetyl taurinate , in particular for magnesium N-acetyl taurinate dihydrate , consisting of:a. a dissolution step (i) of taurine, (ii) of at least one magnesium compound, e.g. magnesium oxide or magnesium hydroxide and (iii) acetic anhydride in water with salt formation and acetylation of the said taurine to generate a solution containing acetylated magnesium taurinate;b. a step of evaporation and/or distillation of said solution obtained in step a) to remove at least some of the excess water and acetic acid and generate a first precipitate, in particular a first precipitate in distillate form, containing the acetylated magnesium taurinate;c. at least one water washing step, e.g. by filtration, of said first precipitate obtained in step b), said water washing step being followed by a step d) of evaporation and/or distillation to remove at least some of the excess water and acetic acid and generate a second precipitate, in particular a second precipitate in distillate form, containing the acetylated magnesium taurinate;e. at least one wash step, with a rinse solution containing ethanol, preferably a rinse solution containing only ethanol, of said second precipitate obtained in step d), said wash step with a rinse solution containing ethanol, preferably a rinse solution containing only ethanol, being followed by a step f) of evaporation and/or distillation to remove at least some of the excess water and ethanol and generate a third precipitate containing the acetylated magnesium taurinate;g. a cooling step of said third precipitate obtained in step f);h. a step of purification and/or washing of said cooled-down third precipitate obtained in step g) to generate a fourth precipitate in cake form; andi. a drying/desiccation step of said purified and/or washed ...

Method for the production of crystalline forms and crystalline forms of optical enantiomers of modafinil

The invention relates to a method for the production of crystalline forms of optical enantiomers of modafinil, comprising the following steps:i) one of the optical enantiomers of modafinil is dissolved in a solvent other than ethanol; ii) the enantiomer of modafinil is crystallized; iii) the crystalline form of the enantiomer of modafinil thus obtained is recovered. The invention also relates to a method for the production of optical enantiomers of modafinil.

Process for the production of 4,4'-dichlorodiphenyl sulfone

A method for the preparation of polymer grade 4,4'-dichlorodiphenyl sulfone (DCDPS) which is substantially free of 2,4' and 3,4'-isomers of dichlorodiphenyl sulfone with yield of over 90%, with substantially reduced reaction times without the use of impregnated catalysts. Furthermore, the reactants and byproducts are substantially recycled. The process involves reacting dimethyl sulfate with sulfur trioxide, reacting the formed dimethyl pyrosulfate with unreacted sulfur trioxide, reacting the mixture with monochlorobenzene, isolating the crude DCDPS using solvent extraction, recovering the solvent from the mother liquor and crystallizing the pure DCDPS. In another aspect, a process in which isomeric mixture of 4,4'-, and 2,4'-dichlorodiphenyl sulfone produced during the preparation of DCDPS is converted to value added products such as diphenyl sulfone, 2,4'- dihydroxydiphenyl sulfone, 4,4'-dihydroxydiphenyl sulfone and 2-aminodiphenyl sulfone.

一种从半导体工业废液中回收二甲基亚砜的方法

本发明涉及一种从半导体工业废液中回收二甲基亚砜的方法，属于废液回收技术领域；二甲基亚砜废液来自半导体工业，首先将二甲基亚砜废液送入刮板膜蒸发器进行减压蒸发，除去颗粒物、光刻胶、碱；然后，再加入水进行混合后，送入间歇精馏塔釜，水与丙二醇甲醚、丙二醇甲醚醋酸酯共沸物，精塔顶首先得到丙二醇甲醚、丙二醇甲醚醋酸酯和水的混合物；再分别得到水和二甲基亚砜混合的过渡馏分、二甲基亚砜成品；本发明利用绿色、无害的水与杂质共沸的特点，去除高附加值废液中的多种杂质，从而达到废液资源综合利用的目的，具有较高的经济效益以及环保价值。

A PROCESS FOR PURIFYING CRUDE 4,4'-DICHLORODIPHENYL SULFONE

The invention relates to a process for purifying crude 4,4′-dichlorodiphenyl sulfone comprising: (a) dissolving the crude 4,4′-dichlorodiphenyl sulfone which may contain water in an organic solvent in which 4,4′-dichlorodiphenyl sulfone has a solubility of 0.5 to 20% at 20° C. and optionally adding water to obtain a solution which comprises 4,4′-dichlorodiphenyl sulfone, the organic solvent and 1 to 30 wt % water based on the amount of 4,4′-dichlorodiphenyl sulfone and water; (b) cooling the solution to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfone to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfone; (c) carrying out a solid-liquid separation to obtain residual moisture containing 4,4′-dichlorodiphenyl sulfone and a mother liquor; (d) washing the residual moisture containing 4,4′-dichlorodiphenyl sulfone with an organic solvent in which 4,4′-dichlorodiphenyl sulfone has a solubility of 0.5 to 20% at 20° C.; (e) optionally repeating steps (b) to (d); (f) drying the 4,4′-dichlorodiphenyl sulfone. 116.-. (canceled)17. A process for purifying crude 4 ,4′-dichlorodiphenyl sulfone comprising:(a) obtaining a solution which comprises 4,4′-dichlorodiphenyl sulfone, an organic solvent, in which 4,4′-dichlorodiphenyl sulfone has a solubility of 0.5 to 20% at 20° C., and 1 to 30 wt % water based on the amount of 4,4′-dichlorodiphenyl sulfone and water by dissolving the crude 4,4′-dichlorodiphenyl sulfone which optionally contains water in the organic solvent and optionally adding water;(b) cooling the solution to a temperature below the saturation point of 4,4′-dichloro-diphenyl sulfone to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfone;(c) carrying out a solid-liquid separation to obtain residual moisture containing 4,4′-di-chlorodiphenyl sulfone and a mother liquor;(d) washing the residual moisture containing 4,4′-dichlorodiphenyl sulfone with an organic solvent in which 4,4′-dichlorodiphenyl ...

Process

Process

파라-하이드로퀴논 유도체의 제조방법

본 발명은 항산화 및 심장기능 강화 등의 활성을 보유하여 화장품, 의약 및 건강보조식품 등의 원료로 광범위하게 사용되는 코엔자임 Q10의 제조를 위한 중간체인 하기 화학식 1의 파라-하이드로퀴논 유도체를 제조하는 방법에 관한 것이다. (화학식 1) 상기식에서, R은 C 1 내지 C 4 알킬을 나타내고, R 1 은 메틸 그룹에 의해 치환되거나 비치환된 탄소수 6개의 방향족 탄화수소를 나타낸다. 코엔자임 Q10, 파라-하이드로퀴논 유도체

아렌설포닉 에시드로부터 아렌설포닐 클로라이드를 얻는 새로운 방법

본 발명은 정밀화학 분야의 핵심적 중간체들의 합성과정에서 관능기 들의 변환에 중요한 역할을 하는 아릴설포닐 클로라이드의 새로운 제조 방법에 관한 것으로, 이전의 기술들이 아릴설포닉 에시드로 부터 아릴설포닐 클로라이드를 제조하는 방법으로 제시했던 섭시 70도 이상의 고온 반응과 긴 반응시간 및 균일하지 못한 반응조건 등의 문제점들을 해결하기 위해 아릴설포닉 에시드를 비스(트리클로로메틸)카보네이트 와 제삼인산칼륨 및 촉매량의 트리에틸아민과 섭시25도 이하의 온화한 조건에서 반응시킴을 특징으로 하는 아릴설포닐 클로라이드를 고수율로 얻는 새로운 방법을 제공함으로써 염료, 농약, 의약 및 전자재료등 관련 산업분야의 발전에 크게 기여할 것이다.

반응 증류를 이용한 3-머캅토프로피온산의 제조 방법

본 발명은 3-머캅토프로피온산의 제조 방법에 관한 것이다. 본 발명에 따르면, 반응 증류를 이용하여 보다 단순화된 공정과 우수한 반응 효율로 3-머캅토프로피온산을 대량 생산할 수 있는 제조 방법이 제공된다.

纯化甲基磺草酮的方法

公开了一种降低甲基磺草酮样品中氰化物水平的方法，所述方法包括：(i)取含水溶剂中的甲基磺草酮样本的水溶液，(ii)调节所述水溶液的pH值至9.5或更高，和(iii)将甲基磺草酮从溶液中结晶出来。

Sulfur-containing compounds as solvents

提供了使用包含短链脂族酯或酰胺部分的含硫化合物作为溶剂的方法以及包含这些化合物的组合物。

METHOD FOR PRODUCING POLYMORPHIC FORMS OF THE MESOTRION

ÐÎÑÑÈÉÑÊÀß ÔÅÄÅÐÀÖÈß (19) RU (11) 2007 110 952 (13) A (51) ÌÏÊ C07C 315/06 (2006.01) ÔÅÄÅÐÀËÜÍÀß ÑËÓÆÁÀ ÏÎ ÈÍÒÅËËÅÊÒÓÀËÜÍÎÉ ÑÎÁÑÒÂÅÍÍÎÑÒÈ, ÏÀÒÅÍÒÀÌ È ÒÎÂÀÐÍÛÌ ÇÍÀÊÀÌ (12) ÇÀßÂÊÀ ÍÀ ÈÇÎÁÐÅÒÅÍÈÅ (21), (22) Çà âêà: 2007110952/04, 03.08.2005 (71) Çà âèòåëü(è): ÇÈÍÃÅÍÒÀ ÏÀÐÒÈÑÈÏÅÉØÍÑ Àà (CH) (30) Êîíâåíöèîííûé ïðèîðèòåò: 26.08.2004 GB 0419075.7 (43) Äàòà ïóáëèêàöèè çà âêè: 10.10.2008 Áþë. ¹ 28 (87) Ïóáëèêàöè PCT: WO 2006/021743 (02.03.2006) Àäðåñ äë ïåðåïèñêè: 101000, Ìîñêâà, Ì.Çëàòîóñòèíñêèé ïåð., 10, êâ.15, "ÅÂÐÎÌÀÐÊÏÀÒ", ïàò.ïîâ. È.À.Âåñåëèöêîé R U (57) Ôîðìóëà èçîáðåòåíè 1. Ñïîñîá ñåëåêòèâíîãî ðåãóëèðîâàíè êðèñòàëëèçàöèè òåðìîäèíàìè÷åñêè ñòàáèëüíîé ôîðìû 1 èëè êèíåòè÷åñêè ñòàáèëüíîé ïîëèìîðôíîé ôîðìû 2 ìåçîòðèîíà èç âîäíîãî ðàñòâîðà ìåçîòðèîíà, óêàçàííûé ñïîñîá âêëþ÷àåò èçìåíåíèå ðÍ ðàñòâîðà ìåçîòðèîíà äî çíà÷åíè , ïðè êîòîðîì â êîíå÷íîì ñ÷åòå ïîëó÷àåòñ òåðìîäèíàìè÷åñêè ñòàáèëüíà ôîðìà 1 èëè êèíåòè÷åñêè ñòàáèëüíà ôîðì 2 ìåçîòðèîíà. 2. Ñïîñîá ïî ï.1, â êîòîðîì çíà÷åíèå ðÍ ðàñòâîðà ìåçîòðèîíà ñíà÷àëà óâåëè÷èâàþò äî ðÍ≥7. 3. Ñïîñîá ïî ï.1, â êîòîðîì çíà÷åíèå ðÍ äîâîä ò äî ≤3,0, ÷òî ïðèâîäèò ê ïîëó÷åíèþ òåðìîäèíàìè÷åñêè ñòàáèëüíîé ôîðìû 1 ìåçîòðèîíà. 4. Ñïîñîá ïî ï.1, â êîòîðîì çíà÷åíèå ðÍ äîâîä ò äî ïðåâûøàþùåãî 3,0, ÷òî ïðèâîäèò ê ïîëó÷åíèþ êèíåòè÷åñêè ñòàáèëüíîé ôîðìû 2 ìåçîòðèîíà. 5. Ñïîñîá ïî ï.1, â êîòîðîì óìåíüøåíèå çíà÷åíè ðÍ ïðîâîä ò ïóòåì ïðèáàâëåíè êèñëîòû ê ðàñòâîðó ìåçîòðèîíà. 6. Ñïîñîá ïî ï.1, â êîòîðîì äë ñîäåéñòâè êðèñòàëëèçàöèè ôîðìû 1 ê ðàñòâîðó ïîñëå ðåãóëèðîâàíè çíà÷åíè ðÍ ïðèáàâë þò çàòðàâî÷íûå êðèñòàëëû ôîðìû 1. 7. Ñïîñîá ïî ï.1, â êîòîðîì óêàçàííûé ñïîñîá îñóùåñòâë þò ïðè òåìïåðàòóðå ≥25°Ñ. 8. Ñïîñîá ïðåâðàùåíè ôîðìû 2 ìåçîòðèîíà â ôîðìó 1 ìåçîòðèîíà, óêàçàííûé ñïîñîá âêëþ÷àåò óìåíüøåíèå çíà÷åíè ðÍ ñóñïåíçèè ôîðìû 2 ìåçîòðèîíà äî ðÍ≤3,0. 9. Ñïîñîá ïî ï.8, â êîòîðîì ôîðìó 2 ìåçîòðèîíà ïðåäâàðèòåëüíî âûäåë þò è ïîâòîðíî ñóñïåíäèðóþò â ïîäõîä ùåì ðàñòâîðèòåëå. 10. Ñïîñîá ïî ï.8, â êîòîðîì ôîðìà 2 ìåçîòðèîíà îáðàçîâàëàñü â òåõíîëîãè÷åñêîì öèêëå è óæå ...

Production method of high-purity diphenyl sulfone

本发明公开了一种高纯度二苯砜的生产方法，包括如下步骤：取一定量的苯，加入离子液，在一定温度下，再加入氯磺酸，在搅拌条件下，苯和氯磺酸进行反应；以离子液富集的氯化氢为催化剂，苯和氯磺酸进行“一锅法”反应，得到粗品二苯砜；反应完全后，用冷水或碎冰淬灭反应，抽滤或离心后得到粗品二苯砜；采用有机溶剂溶解粗品二苯砜，再分别使用碱液、乙二胺四乙酸四钠盐水溶液进行洗涤，得到二苯砜有机溶液；将二苯砜有机溶液利用活性炭脱色，过滤除去活性炭，得到的滤液，再经冷却析晶、抽滤或离心、干燥，得到二苯砜产品。该方法反应条件温和，收率优良，生产工艺简单方便，安全可靠，且比较环保，杂质去除效率高，所获得的产品纯度可高达99.9％。

Method for separating dimethyl sulfoxide from amlodipine resolution waste liquid

本发明涉及溶剂的分离回收技术领域，具体公开一种从氨氯地平拆分废液中分离二甲基亚砜的方法，具体为：用聚酰亚胺纳滤膜对氨氯地平拆分废液进行纳滤，得到的纳滤清液即为回收的二甲基亚砜；所述聚酰亚胺纳滤膜在二甲基亚砜中的溶胀比为1.4‑1.6，截留精度为180‑200Da。本发明的回收方法简单，大大降低二甲基亚砜的回收成本，并显著提高了二甲基亚砜的回收率和纯度。

Crystal Form and Method for Preparation of Crystal Form of Optical Enantiomers of Modafinil

본 발명은 다음의 단계들을 포함하는 모다피닐의 광학 거울상 이성질체들의 결정체 형태의 제조 방법에 관한 것이다: i) 모다피닐의 광학 거울상 이성질체들 중 하나를 에탄올 이외의 용매에 용해시키는 단계; ii) 상기 모다피닐의 거울상 이성질체를 결정화시키는 단계; iii) 그렇게 하여 얻어진 상기 모다피닐의 거울상 이성질체의 결정체 형태를 회수하는 단계. 본 발명은 또한, 모다피닐의 광학 거울상 이성질체들의 제조 방법에 관한 것이다 The present invention relates to a process for the preparation of crystalline forms of optical enantiomers of modafinil including the following steps: i) dissolving one of the optical enantiomers of modafinil in a solvent other than ethanol; ii) crystallizing the enantiomer of said modafinil; iii) recovering the crystalline form of the enantiomer of modafinil thus obtained. The invention also relates to a process for the preparation of optical enantiomers of modafinil. 모다피닐, 광학, 거울상 이성질체, 결정체, 제조방법 Modafinil, Optics, Enantiomers, Crystals, Manufacturing Method

METHOD OF CRYSTALLIZATION OF THE MESOTRION

1. Способ селективного регулирования кристаллизации полиморфной формы 1 мезотриона из водного раствора мезотриона, указанный способ включает применение полунепрерывного или непрерывного способа кристаллизации, в котором водный раствор мезотриона вводят в кристаллизатор, содержащий затравочные кристаллы преимущественно формы 1 в полунепрерывном или непрерывном режиме, и в котором в конечном счете получают указанную форму 1 мезотриона. ! 2. Способ по п.1, в котором значение pH раствора мезотриона увеличивают до равного >7 до его прибавления в кристаллизатор. ! 3. Способ по п.2, в котором раствор мезотриона прибавляют в кристаллизатор при поддержании значения pH в кристаллизаторе равным 4,0 или менее. ! 4. Способ по п.3, в котором значение pH в кристаллизаторе поддерживают путем прибавления кислоты к раствору мезотриона. ! 5. Способ по п.1, в котором указанную кристаллизацию проводят при температуре, равной ≥25°С. ! 6. Способ превращения формы 1 мезотриона в форму 2 мезотриона, указанный способ включает введение раствора, содержащего форму 2 мезотриона, в кристаллизатор, содержащий затравочные кристаллы преимущественно формы 1 в полунепрерывном или непрерывном режиме, и в котором в конечном счете получают указанную форму 1 мезотриона. ! 7. Способ по п.6, в котором форма 2 мезотриона образовалась при осуществлении технологии и уже была суспендирована в полученном маточном растворе. ! 8. Способ по п.6, в котором значение pH раствора формы 2 мезотриона увеличивают до равного >7 до прибавления в кристаллизатор. ! 9. Способ по п.6, в котором значение pH в кристаллизаторе поддерживают путем прибавления кислоты к раствору мезотриона. ! 10. Способ п РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) 2008 133 475 (13) A (51) МПК C07C 315/06 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ, ПАТЕНТАМ И ТОВАРНЫМ ЗНАКАМ (12) ЗАЯВКА НА ИЗОБРЕТЕНИЕ (71) Заявитель(и): ЗИНГЕНТА ПАРТИСИПЕЙШНС АГ (CH) (21), (22) Заявка: 2008133475/04, 15.01.2007 (30) Конвенционный приоритет: 18.01. ...

Preparation method of water-soluble florfenicol amino acid salt

本发明公开了一种水溶性氟苯尼考氨基酸酯盐的制备方法，所述方法，以氟苯尼考和N‑Cbz‑氨基酸为起始原料，经过酰氯化、酯化、脱保护和酸化成盐反应，得到水溶性的氟苯尼考氨基酸酯盐。本发明中原料商业可得、成本低，反应过程中各单元反应条件温和可控，收率高，得到的氟苯尼考氨基酸酯盐纯度高、水溶性好，适用于水溶性氟苯尼考氨基酸酯盐的大规模生产应用。

Method for distilling dimethyl sulfoxide and multi-section distillation tower

本发明涉及蒸馏二甲亚砜的方法，是使用蒸馏装置蒸馏包含二甲亚砜的液体的方法，其包含下述步骤：(1)在蒸馏装置底部的包含二甲亚砜的液体中，按照相对于蒸馏装置底部的包含二甲亚砜的液体、碳酸钠的总计100重量％、碳酸钠为0.005重量～25重量％那样混合碳酸钠，进行加热，(2)从与加入包含二甲亚砜的液体的位置相比靠下部、并且与加热部相比靠上部的位置，获得包含二甲亚砜的馏分。本发明涉及多段式蒸馏塔，是蒸馏包含二甲亚砜的液体的多段式蒸馏塔。通过本发明的多段式蒸馏塔而回收/精制的二甲亚砜的杂质少，纯度高。

Novel Bis(methyl-halo-phenylsulfonyl)diazomethanes and their preparation

본 발명은 화학증폭에 바탕을 둔 반도체용 초미세가공 재료의 일부로서 초고집적반도체 등의 반도체 디바이스를 제작하는데 있어 기판을 미세하게 가공하는 프로세스에 사용되어 광 또는 엑스선, 전자선등의 조사에 의해 미세화상의 패턴을 얻는 용도로 쓰이는 광산발생제로 사용되는 신규물질 및 그 제조방법에 관한 것이다.

A kind of preparation method of deuterated dimethyl sulfoxide

本发明公开了一种氘代二甲基亚砜的制备方法，该方法为：以二甲基亚砜和重水为原料，加入碱催化剂，在90‑95℃下反应1‑3小时，然后升温至130‑150℃分离出水分；继续向反应液中加入重水，重复以上反应操作2‑5次；将反应液减压蒸馏，收集100‑110℃的馏分，得到氘代二甲基亚砜粗品。将所述氘代二甲基亚砜粗品在16‑18℃的环境下进行重结晶，低温过滤得到精制的氘代二甲基亚砜，经高分辨质谱检测其氘代度大于99.8％。

Process for producing methanesulfonic acid

本发明涉及一种通过使自由基引发剂组合物与甲烷和三氧化硫反应而制造甲磺酸的方法，包括下列步骤：(a)通过使过氧化氢水溶液与组分甲磺酸和甲磺酸酐反应而制备所述引发剂组合物，和(b)使来自步骤(a)的引发剂组合物与三氧化硫和甲烷反应而形成甲磺酸。本发明进一步涉及甲磺酸酐(MSA酸酐)在所述方法中的用途以及由所述方法制造的甲磺酸。

The method for preparing high-purity 4,4 '-dichloro diphenyl sulfone

本发明公开了一种制备高纯度4,4′–二氯二苯砜的方法。该方法以亚砜氧化法生产的4,4’‑二氯二苯砜初产品为原料，以甲苯为溶剂，通过加入氢氧化钠水溶液与冰醋酸及硫酸等无机酸性杂质反应，EDTA四钠盐与Al 3+ 和Fe 3+ 等金属离子络合，活性炭吸附有机色素杂质等，低温冷却重结晶，制备高纯度4,4’‑二氯二苯砜。反应除杂温度105‑110℃，反应除杂时间4‑6小时，重结晶冷却温度为零下5‑10℃，结晶时间为5‑8小时，高纯度4,4’‑二氯二苯砜的色谱含量为99.95%‑99.99%。本发明方法具有反应条件温和，杂质去除效率高，重结晶收率高，4,4’‑二氯二苯砜纯度高，重结晶溶剂可回收循环使用的优点。

Production method of high-purity diphenyl sulfone

本发明公开了一种高纯度二苯砜的生产方法，包括如下步骤：取一定量的苯，加入离子液，在一定温度下，再加入氯磺酸，在搅拌条件下，苯和氯磺酸进行反应；以离子液富集的氯化氢为催化剂，苯和氯磺酸进行“一锅法”反应，得到粗品二苯砜；反应完全后，用冷水或碎冰淬灭反应，抽滤或离心后得到粗品二苯砜；采用有机溶剂溶解粗品二苯砜，再分别使用碱液、乙二胺四乙酸四钠盐水溶液进行洗涤，得到二苯砜有机溶液；将二苯砜有机溶液利用活性炭脱色，过滤除去活性炭，得到的滤液，再经冷却析晶、抽滤或离心、干燥，得到二苯砜产品。该方法反应条件温和，收率优良，生产工艺简单方便，安全可靠，且比较环保，杂质去除效率高，所获得的产品纯度可高达99.9％。

Method foe preparing high-purity 4,4'-dichlorodiphenyl sulfone

本发明公开了一种制备高纯度4,4’‑二氯二苯砜的方法。该方法以亚砜氧化法生产的4,4’‑二氯二苯砜初产品为原料，以甲苯为溶剂，通过加入氢氧化钠水溶液与冰醋酸及硫酸等无机酸性杂质反应，EDTA四钠盐与Al 3+ 和Fe 3+ 等金属离子络合，活性炭吸附有机色素杂质等，低温冷却重结晶，制备高纯度4,4’‑二氯二苯砜。反应除杂温度105‑110℃，反应除杂时间4‑6小时，重结晶冷却温度为零下5‑10℃，结晶时间为5‑8小时，高纯度4,4’‑二氯二苯砜的色谱含量为99.95%‑99.99%。本发明方法具有反应条件温和，杂质去除效率高，重结晶收率高，4,4’‑二氯二苯砜纯度高，重结晶溶剂可回收循环使用的优点。

Chemenzyme Methods for Co-generation of Disulfides and Sulfoxides or Sulfones

본 발명은 1) 설파이드, 2) 임의적으로 산화제, 3) 적어도 하나의 티올 모이어티를 보유하는 유기 화합물, 4) 상기 설파이드의 설폭사이드 또는 설폰으로의 산화를 촉매하는 효소 E, 5) 이량체를 형성하기 위해 적어도 하나의 티올 모이어티를 보유하는 상기 유기 화합물의 두 등가물 사이에 디설파이드 가교의 형성을 촉매하는 효소 D, 및 6) 두 효소 E 및 D에 공통적인 보조인자를 포함하는 조성물 M으로부터 디설파이드 및 설폭사이드 또는 설폰을 공동생성하기 위한 화학효소적 방법; 및 또한 특히 이러한 방법의 구현을 가능하게 하는 조성에 관한 것이다. 본 발명은 또한 적어도 하나의 티올 모이어티를 보유하는 상기 유기 화합물의 두 등가물 사이에 형성된 디설파이드 가교를 환원시키기 위한 메르캅탄의 용도, 및 더욱 특히, 상기 기재된 방법의 재생 기질로서 이의 용도에 관한 것이다.

Crystalline forms of optical enantiomers of modafinil and method for the procution same

本发明涉及一种制备莫达非尼旋光对映异构体的晶形的方法，包括下列步骤：i)将莫达非尼其中一个旋光对映异构体溶于除乙醇之外的溶剂中；ii)使莫达非尼的对映异构体结晶；iii)回收所得莫达非尼对映异构体的晶形。本发明还涉及一种制备莫达非尼旋光对映异构体的方法。

Purification of 2-nitro-4-methylsulfonylbenzoic acid

FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to a method for purifying 2-nitro-4-methylsulfonylbenzoic acid from impurities. Method involves at least two of the following steps in any order: (a) dissolving 2-nitro-4-methylsulfonylbenzoic acid in water at pH about 3-7 followed by filtration; (b) contacting 2-nitro-4-methylsulfonylbenzoic acid aqueous solution with activated carbon at pH about 2-10; (c) treatment of 2-nitro-4-methylsulfonylbenzoic acid aqueous solution with the sufficient amount of a base for hydrolysis of unfavorable nitro- and dinitro-substituted impurities. Then the prepared aqueous solution containing 2-nitro-4-methylsulfonylbenzoic acid is kept at temperature up to about 95°C and pH value of this solution is brought about to pH providing crystallization of 2-nitro-4-methylsulfonylbenzoic acid at cooling. Also, invention describes a method for preparing mesotrion that comprises conversion of purified 2-nitro-4-methylsulfonylbenzoic acid to the corresponding acid chloroanhydride that is subjected to interaction with 1,3-dicyclohexanedione to yield mesotrion. The proposed method can be used in synthesis of herbicide for cereal crops and used for control of grassy and platyphyllous weeds before and after their germination. EFFECT: improved purifying method of compound. 10 cl, 5 ex ÐÎÑÑÈÉÑÊÀß ÔÅÄÅÐÀÖÈß RU (19) (11) 2 287 521 (13) C2 (51) ÌÏÊ C07C 317/24 C07C 317/44 (2006.01) (2006.01) ÔÅÄÅÐÀËÜÍÀß ÑËÓÆÁÀ ÏÎ ÈÍÒÅËËÅÊÒÓÀËÜÍÎÉ ÑÎÁÑÒÂÅÍÍÎÑÒÈ, ÏÀÒÅÍÒÀÌ È ÒÎÂÀÐÍÛÌ ÇÍÀÊÀÌ (12) ÎÏÈÑÀÍÈÅ ÈÇÎÁÐÅÒÅÍÈß Ê ÏÀÒÅÍÒÓ (21), (22) Çà âêà: 2003131328/04, 25.03.2002 (30) Êîíâåíöèîííûé ïðèîðèòåò: 26.03.2001 US 60/275.061 (73) Ïàòåíòîîáëàäàòåëü(è): ÑÈÍÄÆÅÍÒÀ ËÈÌÈÒÅÄ (GB) (43) Äàòà ïóáëèêàöèè çà âêè: 27.01.2005 R U (24) Äàòà íà÷àëà îòñ÷åòà ñðîêà äåéñòâè ïàòåíòà: 25.03.2002 (72) Àâòîð(û): ÄÆÀÂÄÀÍÈ Êàìáèç (US), ÐÎÄÐÈÃÅÑ Ãèëáåðò (US), ÌÀÊÑÂÎÐÒÈ Äæåéìñ Ïèòåð (GB) (45) Îïóáëèêîâàíî: 20.11.2006 Áþë. ¹ 32 2 2 8 7 5 2 1 (56) Ñïèñîê äîêóìåíòîâ, ...

Dialdehyde compound, preparation method thereof, and synthetic method of carotenoids using the same

Provided are a novel dialdehyde compound which is used for the synthesis of a carotene compound, a method for preparing the dialdehyde compound, a diol compound, a method for preparing lycopene by using the dialdehyde compound, and a method for preparing beta-carotene by using the dialdehyde compound. The dialdehyde compound is represented by the formula(3), wherein Ar is a C6-C30 substituted or unsubstituted aryl group or a C2-C30 substituted or unsubstituted heteroaryl group. The dialdehyde compound of the formula(3) is prepared by deprotonating geranyl sulfone and reacting it with a geranyl halide to prepare a sulfone compound; preparing a diol compound from the sulfone compound by the allylic oxidation reaction at both terminals; and oxidizing the two alcohol groups of the diol compound.

Synthesis method of tetrabromobisphenol S

本发明提供了一种四溴双酚S的合成方法，包括步骤如下：(1)将双酚S、二氯甲烷和异丁醇的混合溶剂、水混合，搅拌均匀，在10～30℃下，缓慢双滴加双氧水和溴素，滴加完毕后，升温至35～40℃进行反应；(2)反应结束后，将反应体系降至室温，加入亚硫酸钠溶液中和过量溴素，之后调节体系pH值至6～7，经过滤、洗涤、干燥，得四溴双酚S，过滤所得母液直接循环套用。本发明的制备方法成本低、对环境友好、产品收率及纯度高、安全性高。

Method for preparing 2-(2'-chloroethylsulfonyl)ethylamine HCl salt

본 발명은 하기 화학식 1로 표시되는 2-(2'-클로로에틸술포닐)에틸아민 염산염 (2-(2'-chloroethylsulfonyl)ethylamine HCl salt)의 제조방법에 관한 것으로, 구체적으로 2-아미노에틸 황산수소염과 2-메르캅토에탄올을 무기 염기 존재 하에 반응시킨 후, 염소화 및 산화 반응을 동시에 수행하여 하기 화학식 1의 2-(2'-클로로에틸술포닐)에틸아민 염산염을 제조하는 방법으로서, 본 발명의 방법에 의하면 반응 공정이 단축되고 고수율로 고순도의 2-(2'-클로로에틸술포닐)에틸아민 염산염을 제조할 수 있을 뿐만 아니라 출발물질이 저렴하고 수급이 용이하여 공업적으로 유용하게 적용될 수 있다. The present invention relates to a method for preparing 2- (2'-chloroethylsulfonyl) ethylamine hydrochloride (2- (2'-chloroethylsulfonyl) ethylamine HCl salt) represented by the following Chemical Formula 1, specifically 2-aminoethyl sulfur As a method of preparing 2- (2'-chloroethylsulfonyl) ethylamine hydrochloride of Chemical Formula 1 by reacting an oxyhydrogen salt with 2-mercaptoethanol in the presence of an inorganic base and then simultaneously performing a chlorination and an oxidation reaction, the present invention According to the method, the reaction process can be shortened and high-purity 2- (2'-chloroethylsulfonyl) ethylamine hydrochloride can be prepared with high yield, and the starting material is inexpensive and easy to supply so that it can be applied industrially usefully. Can be.

Purification of 2-nitro-4-methylsulfonylbenzoic acid

Process for recovering and recycling acid catalyst

公开了一种使用包含叔胺或羧酸鎓化合物、改性剂和稀释剂的萃取溶剂由乙醇酸的水性混合物萃取回收酸催化剂的方法。所述酸催化剂（其可以包括强酸例如硫酸、烷基磺酸和氟代烷基磺酸）可以使用水性甲醛反萃回收并且再循环至通过酸催化的甲醛羰基化制备乙醇酸的方法中。还公开了通过酸催化的加氢羧化甲醛制备乙醇酸的方法。

Manufacturing method of organic sulfone

The method for oxidation of sulfoxide

本发明涉及将亚砜氧化成各自的砜的方法，所述方法包括在催化剂的存在下使亚砜与过氧化氢反应，得到包含砜和催化剂的混合物(M)，其中所述催化剂包含作为催化活性物质的多孔含钛硅酸盐。

Method and system for refining medical intermediate

本发明提供了一种医药中间体的精制方法和系统，包括以下步骤：S1、向脱色罐内抽入丙酮、所述医药中间体和吸附材料得到混合物，搅拌回流进行脱色；S2、对脱色后的混合物真空过滤加入到浓缩釜中；S3、对浓缩釜中的混合物进行浓缩，随后搅拌降温，静置至得到结晶产物；S4、将所述结晶产物采用所述丙酮离心洗涤若干次，干燥，精制结束。采用本发明技术方案建立了医药中间体精制生产标准操作规程，规范医药中间体精制的生产操作，有效保证医药中间体精制的纯度的稳定性，避免产品质量不一，有效把控产品质量，适合规模化生产。

Purification method of dimethyl sulfoxide (DMSO)

Purification of 2-nitro-4-methylsulphonylbenzoic acid

一种从2－硝基－4－甲磺酰基苯甲酸中除去杂质的方法，所述方法包括至少两个以下任意顺序的步骤：(a)将2－硝基－4－甲磺酰基苯甲酸溶解在pH值约为2至10的水中，随后过滤；(b)在pH值约为2至10下，使2－硝基－4－甲磺酰基苯甲酸的水溶液与活性炭接触；(c)用足量的碱处理2－硝基－4－甲磺酰基苯甲酸的水溶液，水解不需要的硝基和二硝基取代的杂质；随后将所得的含有2－硝基－4－甲磺酰基苯甲酸的水溶液保持在最高可达约95℃的温度下，并且调节所述溶液的pH值至约为在冷却的情况下足于使2－硝基－4－甲磺酰基苯甲酸发生结晶的pH值。

Method for preparing beta-aminosulfone compound

本发明属于有机化学合成技术领域，具体涉及一种制备β‑氨基砜类化合物的方法。本发明将亚磺酰氯、羟肟和烯烃类化合物在三乙胺的存在下进行加成反应，合成得到β‑氨基砜类化合物。本发明首次实现了利用亚磺酰氯、羟肟与烯烃之间的自由基加成反应合成β‑氨基砜类化合物，填补了现有技术的空白；本发明方法工艺条件温和，流程短，步骤简单，底物适用性广，满足工业生产要求；利用本发明的方法合成β‑氨基砜类化合物，产物收率高，产物的收率可高达86％，且生成的β‑氨基砜类化合物在药物中应用广泛。可见，本发明具有重要的应用价值。

Purifying method for dimethylsulfoxide (DMSO)

为了纯化二甲亚砜(DMSO),让DMSO与多种阳离子交换树脂接触,其中至少一种是SO 3 H或－SO 3 NH 4 型磺酸型树脂,另外一种或多种树脂可以是螯合型树脂。这种得到的DMSO的铁阳离子含量低于1ppb,而钠阳离子含量低于2ppb。

Method for preparing β -carbonyl sulfone

本发明公开了一种制备β‑羰基砜的方法。以α‑羰基重氮化合物和芳基亚磺酸钠为反应底物，以廉价的硝酸银为最优催化剂，1,10‑菲啰啉为配体，过硫酸钾为氧化剂，在乙腈与水的混合溶剂中经过偶联反应得到β‑羰基砜化合物。与现有技术相比较，本发明方法具有以下优点：反应底物范围广，反应时间短，反应产率比较高，反应条件温和等优点。本发明使用无毒无害的试剂为反应原料，对环境没有危害，符合当代绿色化学发展的要求。反应后处理比较简单，便于分离提纯。此外，该反应能够实现克级规模合成，为实际应用奠定基础。

Molecular sieve dehydration system for dimethyl sulfoxide and dehydration method thereof

本发明提供了一种用于二甲基亚砜的分子筛脱水系统，包括精馏塔(1)、第一分子筛脱水塔(2)和第二分子筛脱水塔(2’)、气液分相罐(3)和氮气源；精馏塔用于含水二甲基亚砜溶液的精馏，以分离部分水；两个分子筛脱水塔均连接精馏塔，用于已经分离出部分水的含水二甲基亚砜被吸附以进一步脱水；氮气源连接至两个分子筛脱水塔，用于进行塔内残余的含水二甲基亚砜溶液的置换和排放；气液分相罐与两个分子筛脱水塔分别连接，以进行分子筛脱水塔中被置换或再生的物质的气液分离，并将分离出的氮气送入分子筛脱水塔中循环利用；气液分相罐连接精馏塔，用于将分离出的液相送至精馏塔进行再处理。本发明同时提供了进行二甲基亚砜的分子筛脱水的工艺。

DIMETHYLSULFOXIDE (DMSO) PURIFICATION PROCESS

Chemo-enzymatic process for the co-production of a disulfide and a sulfoxide or a sulfone

Procédé chimio-enzymatique de coproduction d’un disulfure et d’un sulfoxyde ou d’une sulfone La présente invention concerne un procédé chimio-enzymatique de coproduction de disulfure et de sulfoxyde ou de sulfone à partir d’une composition M comprenant : un sulfure,éventuellement un oxydant,un composé organique porteur d’au moins un groupement thiol,une enzyme E catalysant l’oxydation dudit sulfure en sulfoxyde ou en sulfone,une enzyme D catalysant la formation d’un pont disulfure entre deux équivalents dudit composé organique porteur d’au moins un groupement thiol pour former un dimère, etun cofacteur commun aux deux enzymes E et D ; ainsi qu’une composition permettant notamment la mise en œuvre de ce procédé. La présente invention concerne également l’utilisation d’un mercaptan pour la réduction d’un pont disulfure formé entre deux équivalents d’un composé organique porteur d’au moins un groupement thiol, et plus particulièrement son utilisation en tant que substrat de régénération du procédé décrit ci-dessus. Chemo-enzymatic process for the co-production of a disulfide and a sulfoxide or a sulfone The present invention relates to a chemo-enzymatic process for the co-production of disulfide and sulfoxide or sulfone from a composition M comprising: a sulfide, optionally an oxidant, an organic compound carrying at least one thiol group, an enzyme E catalyzing the oxidation of said sulfide to sulfoxide or sulfone, an enzyme D catalyzing the formation of a disulfide bridge between two equivalents of said compound organic bearing at least one thiol group to form a dimer, and a cofactor common to the two enzymes E and D; as well as a composition allowing in particular the implementation of this process. The present invention also relates to the use of a mercaptan for the reduction of a disulphide bridge formed between two equivalents of an organic compound bearing at least one thiol group, and more particularly to its use as a substrate for regeneration of the process ...

Process and apparatus for making ultra-pure dmso

One aspect of this invention relates to processes for solidifying dimethylsulfoxide including a step of partially solidifying a liquid phase including dimethylsulfoxide and one or more impurities, to form a mixture comprising solid dimethylsulfoxide and a liquid residue. In certain embodiments of the processes of the invention, ultra-high purity DMSO that exceeds the purity specifications for U.S.P. grade DMSO can be produced by employing solidification, fractional solidification and/or melt crystallization processes.

Chemo-enzymatic process for the co-production of a disulfide and a sulfoxide or a sulfone

Procédé chimio-enzymatique de coproduction d’un disulfure et d’un sulfoxyde ou d’une sulfone La présente invention concerne un procédé chimio-enzymatique de coproduction de disulfure et de sulfoxyde ou de sulfone à partir d’une composition M comprenant : un sulfure,éventuellement un oxydant,un composé organique porteur d’au moins un groupement thiol,une enzyme E catalysant l’oxydation dudit sulfure en sulfoxyde ou en sulfone,une enzyme D catalysant la formation d’un pont disulfure entre deux équivalents dudit composé organique porteur d’au moins un groupement thiol pour former un dimère, etun cofacteur commun aux deux enzymes E et D ; ainsi qu’une composition permettant notamment la mise en œuvre de ce procédé. La présente invention concerne également l’utilisation d’un mercaptan pour la réduction d’un pont disulfure formé entre deux équivalents d’un composé organique porteur d’au moins un groupement thiol, et plus particulièrement son utilisation en tant que substrat de régénération du procédé décrit ci-dessus. The present invention relates to a chemo-enzymatic process for the co-production of a disulfide and a sulfoxide or a sulfone The present invention relates to a chemo-enzymatic process for the co-production of a disulfide and a sulfoxide or a sulfone from a composition M comprising: a sulfide , optionally an oxidant, an organic compound carrying at least one thiol group, an enzyme E catalyzing the oxidation of said sulphide to sulphoxide or sulphone, an enzyme D catalyzing the formation of a disulphide bridge between two equivalents of said organic compound carrying at least one thiol group to form a dimer, anda cofactor common to both enzymes E and D; as well as a composition allowing in particular the implementation of this process. The present invention also relates to the use of a mercaptan for the reduction of a disulphide bridge formed between two equivalents of an organic compound bearing at least one thiol group, and more particularly to its use as a ...

Crystallization point lowering additive for dimethyl sulfoxide, e.g. during use as paint stripper or surface cleaner, comprises diol and/or triol, especially glycerol

The use of at least one diol and/or triol is claimed as crystallization point lowering additive (I) for dimethyl sulfoxide (DMSO). Independent claims are included for: (1) (I)-containing DMSO formulations (A); (2) a composition (II) for stripping paints, cleaning surfaces or removing graffiti, comprising 10-50 wt. % (A) and 10-50 wt. % medium polarity, non-conventional cosolvent(s) (B) (optionally together with conventional additives such as activators, thickeners, softeners and surfactants); and (3) a method for stripping paints, cleaning surfaces or removing graffiti, involving applying (II) by brushing, leaving (II) in contact with the surface for 30 minutes and removing the residues of the paint, dirt or graffiti using a paint scraper.

PROCESS FOR THE SEPARATION OF 4,4'-DICHLORODIPHENYLSULFONE

DIMETHYLSULFOXIDE (DMSO) PURIFICATION PROCESS

COMPOSITION BASED ON ORGANIC SULFIDE WITH MASKED ODOR

Isolation of 4, 4'-dihydroxy-diphenylsulfone from mixtures of this body with the 2, 4'-dihydroxy-diphenylsulfone isomer

PROCESS FOR PURIFYING DIMETHYLSULFOXIDE (DMSO)

Pour purifier un diméthylsulfoxyde (DMSO), on le met en contact avec une pluralité de résines échangeuses de cations dont l'une au moins est une résine de type sulfonique sous forme -SO3 H ou -SO3 NH4, l'autre ou les autres pouvant être de type chélatant.Le DMSO ainsi obtenu a une teneur en cation fer inférieure à 1 ppb et une teneur en cation sodium inférieure à 2 ppb. To purify a dimethylsulfoxide (DMSO), it is brought into contact with a plurality of cation exchange resins, at least one of which is a sulfonic type resin in the form -SO3 H or -SO3 NH4, the other or others being able to be of the chelating type. The DMSO thus obtained has an iron cation content of less than 1 ppb and a sodium cation content of less than 2 ppb.

DIMETHYLSULFOXIDE (DMSO) PURIFICATION PROCESS

Purification method of 4,4'-dichlorodiphenyl sulfone

본 발명은 (a) 카복실산 중 미립자 4,4'-디클로로디페닐 설폰을 포함하는 현탁액을 제공하는 단계, (b) 현탁액의 고체-액체 분리를 수행하여 잔류 수분 함유 4,4'-디클로로디페닐 설폰 및 카복실산을 포함하는 여액을 수득하는 단계, (c) 잔류 수분 함유 4,4'-디클로로디페닐 설폰을 수성 염기에 이어 물로 세척하는 단계, (d) 세척에 사용된 후의 수성 염기를 강산과 혼합하거나, 세척에 사용된 후의 수성 염기를 카복실산을 포함하는 여액 및 강산과 혼합하는 단계, (e) 수성상 및 카복실산을 포함하는 유기상이 수득되는 상 분리를 수행하는 단계를 포함하는 4,4'-디클로로디페닐 설폰의 정제 방법에 관한 것이다.

Alliin extraction process optimization method

本发明提供一种蒜氨酸提取工艺优化方法，涉及化合物提取技术领域，包括如下步骤：S1.大蒜的预处理；S2.提取分离：将储罐中的溶剂通过离心泵导入提取罐中，密封储罐，调节减压阀，打开氮气瓶的第一阀门通过向提取罐中充入氮气达到设定压力后进行保压提取，打开第二阀门排出提取液；S3.浓缩结晶：将提取液倒入减压蒸馏浓缩罐中，将浓缩液使用超滤膜过滤除去胶状物，将过滤液通过离子交换柱进行纯化；S4.溶剂的回收：减压蒸馏浓缩罐中的溶剂注入精馏塔中，精馏后得到95％乙醇并收集；S5.洗脱液的处理：经过减压蒸馏浓缩罐减压蒸馏后的洗脱液进行中和反应后，进行收集或排入下水道。本发明化学污染小，操作方便，成本低，效率高，提取率高，再现性好。

Method for obtaining 4, 4' -dichlorodiphenyl sulfone

本发明涉及一种从包含4,4’‑二氯二苯砜和作为有机溶剂的直链C 6 至C 10 羧酸的有机混合物中获得4,4’‑二氯二苯砜的方法，包括：(a)通过以下方式冷却有机混合物：(a1a)将有机混合物与水在结晶容器中混合，以获得液体混合物；(a1b)通过以下方式将在(a1a)中获得的液体混合物冷却至低于4,4’‑二氯二苯砜饱和点的温度：(i)将结晶容器中的压力降低至水开始蒸发的压力，(ii)通过冷却使蒸发的水冷凝，(iii)将冷凝水混入结晶容器中的液体混合物中，以获得包含结晶4,4’‑二氯二苯砜的悬浮液；或通过以下方式冷却有机混合物：(a2)将有机混合物与至少一个可冷却表面接触，从而以5至50K/h的冷却速率降低有机混合物的温度，直至达到10至30℃的温度，其中有机混合物和至少一个可冷却表面具有温差，其在整个冷却过程中保持在1至30K的范围内，以获得包含结晶4,4’‑二氯二苯砜的悬浮液；(b)将(a1b)或(a2)中得到的悬浮液进行固液分离，以获得含残留水分的固体4,4’‑二氯二苯砜作为产品，以及包含有机溶剂和水的母液。

Dimethylsulfoxide (dmso) purification process

Pour purifier un diméthylsulfoxyde (DMSO), on met ce DMSO en contact avec une résine échangeuse d'ions de type sulfonique sous forme -SO3NH4, puis on sépare le DMSO de la résine. Le DMSO ainsi obtenu a une teneur en cation fer inférieure à 1 ppb, une teneur en cation sodium inférieure à 2 ppb, et il est particulièrement adapté notamment par une utilisation dans l'industrie pharmaceutique et électronique. To purify a dimethyl sulfoxide (DMSO), this DMSO is brought into contact with an ion-exchange resin of sulfonic type in the form -SO3NH4, then the DMSO is separated from the resin. The DMSO thus obtained has an iron cation content of less than 1 ppb, a sodium cation content of less than 2 ppb, and it is particularly suitable in particular for use in the pharmaceutical and electronic industry.

Method for purifying dimethyl sulfoxide

Method for purifying dimethyl sulfoxide

本发明是一种二甲亚砜的纯化方法，在惰性气体环境中在碳酸钠的存在下对含二甲亚砜液体进行蒸馏，从而蒸馏出二甲亚砜，蒸馏后的残液中碳酸钠的量相对于二甲亚砜净量100g的相对量是蒸馏前含二甲亚砜液体中碳酸钠的量相对于二甲亚砜净量100g的6倍以上。本发明的二甲亚砜的纯化方法，不仅蒸馏后的馏出液(主馏分和前馏分)，而且在蒸馏后的残液中二甲亚砜的分解也少。蒸馏后的残液、或蒸馏中的液体中二甲亚砜的分解少，所以能够通过蒸馏得到高纯度的二甲亚砜。

Process for purifying mesotrione

A process for reducing the levels of undesirable impurities in a mesotrione sample is disclosed, said process comprising the steps of: (i) forming a mesotrione enolate solution in an aqueous solvent, (ii) carrying out one or more purification processes, and (iii) crystallising the purified mesotrione out of solution.

Crystalline form of the optical enantiomers of modafinil

Production of crystalline forms (specifically polymorphic forms or solvates) of enantiomers of modafinil (A) involves dissolving an enantiomer of (A) (preferably the levorotatory isomer, (-)-(A)) in a solvent other than ethanol, crystallizing the enantiomer and recovering the obtained crystalline form. Some polymorphic forms and solvates of (-)-(A) are new. Independent claims are included for: (a) the following new polymorphic forms of (-)-(A): (i) Form II, having an X-ray diffraction pattern with maxima corresponding to interplanar spacings of 8.54Å, 7.57Å, 7.44Å, 4.56Å, 3.78Å and 3.71Å; (ii) Form III, having an X-ray diffraction pattern with maxima corresponding to interplanar spacings of 12.58Å, 8.54Å, 5.01Å, 4.10Å, 3.97Å and 3.20Å; and (iii) Form IV, having an X-ray diffraction pattern with maxima corresponding to interplanar spacings of 12.38Å, 8.58Å, 7.34Å, 5.00Å and 4.09Å; (b) a new dimethyl carbonate solvate of (-)-(A), having an X-ray diffraction pattern with maxima corresponding to interplanar spacings of 12.31Å, 9.69Å, 9.09Å, 8.54Å, 7.27Å, 6.21Å, 5.45Å, 5.10Å, 5.00Å, 4.83Å, 4.63Å, 4.46Å, 4.22Å, 4.21Å, 4.09Å, 3.78Å, 3.62Å, 3.53Å, 3.42Å, 3.32Å, 3.24Å, 3.21Å and 3.10Å; (c) a method for converting a first crystalline form of an enantiomer of (A) (specifically Form I of (-)-(A)) into another crystalline form, involving suspending the first crystalline form in a suitable solvent and recovering the second form (the solvate specifically being acetonitrile, with the product being recovered as acetonitrile solvate); (d) a new acetonitrile solvate of (-)-(A), having an X-ray diffraction pattern with maxima corresponding to interplanar spacings of 16.17Å, 14.14Å, 12.32Å, 10.66Å, 9.79Å, 9.29Å, 8.54Å, 8.15Å, 7.80Å, 7.09Å, 6.31Å, 5.83Å, 5.62Å, 5.41Å, 5.10Å, 4.90Å, 4.66Å, 4.58Å, 4.46Å, 4.33Å, 4.20Å, 4.02Å, 3.92Å, 3.835Å, 3.72Å, 3.60Å, 3.57Å, 3.45Å, 3.33Å, 3.24Å, 3.19Å, 3.0Å and 3.03Å; (e) the preparation of optically active (A) from modafinic acid (B) by: (i) optically ...

Novel preparation method for preparing florfenicol crystal

本发明公开了一种制备氟苯尼考晶体的新型制备方法，包括在反应釜内，加入溶剂四氢呋喃，将氟苯尼考原粉溶于四氢呋喃中，配制成浓度为30mg/ml‑80mg/ml的四氢呋喃溶液，在另一反应釜内，配制反溶剂水溶液等步骤。本发明采用了反溶剂法重结晶得到氟苯尼考超微粉的方法，有两大优点，一是采用含透明质酸钠/乙醇的水溶液，具有特别优良的超微效果，二是采用了对冲射流出口，更加强化了液滴之间的碰撞，有利于液滴的破碎，有利于实现超微化效果。

Method for synthesizing 4, 4' -dichlorodiphenyl sulfone by solid acid catalysis

本发明涉及苯砜技术领域，具体涉及一种固体酸催化合成4,4´‑二氯二苯砜的方法。本发明所述的固体酸催化合成4,4´‑二氯二苯砜的方法，是将4,4´‑二氯二苯亚砜、固体酸催化剂和溶剂混合升温，然后滴加过氧化氢，反应完全后，分离，将反应液进行后处理，得到所述的4,4´‑二氯二苯砜和水油两相混合液。本发明设计科学合理，采用的催化剂的单体来源广泛，适用于多种溶剂体系，易于从反应体系分离回用，反应后的溶剂可回收使用，对环境无污染，对设备无腐蚀，目标产物的纯度高、收率高。

Preparation methods of crystalline forms of optical enantiomers of modafinil and pharmaceutical composition therof

L'invention a pour objet un procédé de préparation de formes cristallines des énantiomères optiques du modafinil, comprenant les étapes consistant à :i) dissoudre l'un des énantiomères optiques du modafinil dans un solvant autre que l'éthanol ;ii) cristalliser l'énantiomère du modafinil ;iii) récupérer la forme cristalline de l'énantiomère du modafinil ainsi obtenue. L'invention vise également un procédé de préparation des énantiomères optiques du modafinil. The invention relates to a process for the preparation of crystalline forms of the optical enantiomers of modafinil, comprising the steps of: i) dissolving one of the optical enantiomers of modafinil in a solvent other than ethanol, ii) crystallizing the enantiomer of modafinil, iii) recovering the crystalline form of the enantiomer of modafinil thus obtained. The invention also relates to a process for preparing the optical enantiomers of modafinil.

Modafinil polymorphic forms