ДИСОЛИ МАЛОНОВОЙ КИСЛОТЫ И СПОСОБ ПОЛУЧЕНИЯ МАЛОНИЛДИГАЛОГЕНИДОВ

Изобретение относится к способу получения соединения формулы 1, где Rпредставляет собой фенил, замещенный 1 или 2 заместителями, независимо выбранными из Cl или CF; и X представляет собой Cl или Br, включающему приведение в контакт соединения формулы 2, где Rпредставляет собой фенил, замещенный 1 или 2 заместителями, независимо выбранными из Cl или CF; и каждый Mи Mнезависимо представляет собой Na, K, NH, NH(CHCH)или NH(СНСНСНСН), с галогенирующим средством. Предложенный способ является более коротким и более эффективным. 2 з.п. ф-лы, 3 пр., 321 табл.

ЗАМЕЩЕННЫЕ КАРБОКСАМИДЫ И ФАРМАЦЕВТИЧЕСКАЯ КОМПОЗИЦИЯ НА ИХ ОСНОВЕ

Замещенные карбоксамиды формулы I, где R1 - меркапто, ацетилтио, карбокси, гидроксикарбамоил, C1-C4-алкоксикарбонил, ар-(C1-C4)-алкоксикарбонил, бензилоксикарбамоил или -PO(OH)CH2SR6, R6 - хинолил, нафтил, пиридил или фенил, R2 - алкил, циклоалкил-C1-C4-алкил или аралкил; R3 - циклоалкил-C1-C4 алкил, возможно замещенный гидрокси, алкилтио, пиридилом или индолилом; R4 - нитро, амино, циано, гидрокси, алкокси, алкоксикарбонилалкил, тетразолил, карбамоил; R5 - водород или гидрокси, в виде отдельного стериоизомера или их смеси или его фармацевтически приемлемая соль, обладают способностью ингибировать матричные металлопротеазы. 2 с. и 14 з.п.ф-лы.

СПОСОБ ПОЛУЧЕНИЯ ХЛОРАНГИДРИДОВ КАРБОНОВЫХ КИСЛОТ

Использование: в основном органическом синтезе. Сущность изобретения: продукт: хлорангидрид монохлоруксусной кислоты. БФ C2H2 Cl2O, выход 87 90% Хлорангидрид пропионовой кислоты, БФ C3H5ClO, выход 86% Хлорангидрид α хлорпропионовой кислоты, БФ C3H4Cl2O, выход 90% Реагент 1: карбоновая C1-C3 кислота. Реагент 2: газообразный хлор. Условия реакции: при нагревании в присутствии хлористой серы и вторичного или третичного амина в количестве 0,02 0,06 моль на 1 моль карбоновой кислоты под избыточным давлением 0,01 0,1 МПа. 1 табл.

Способ получения хлорангидридов карбоновых кислот

Использование: в основном органическом синтезе . Сущность изобретения: продукт: хлорангид- рид монохлоруксусной кислоты. БФ С Н CI О, выход 87 - 90%. Хлорангидрид пропионовои кислоты, БФ С Н СЮ, выход 8696. Хлорангидрид а хлорп- ропионовой кислоты, БФ С Н CI О, выход 90%. Реагент 1: карбоновая С -С - кислота. Реагент12: газообразный хлор. Условия реакции: при нагревании в присутствии хлористой серы и вторичного или третичного амина в количестве 0.02 - 0.06 моль на 1 моль карбоновой кислоты под избыточным давлением 0,01 - 0,1 МПа 1 табл.

Способ получения роксалилхлорида

Способ получения фторангидридов перфторкарбоновых или сульфокислот

Способ очистки отходящих газов производства хлористого бензоила

Инсектицидное средство в форме эмульгируемого концентрата

ИНСЕКТИЦИДНОЕ СРЕДСТВО В ФОРМЕ ЭМУЛЬГИРУЕМОГО-КОНЦЕНТРАТА, содержащее активный ингредиент производное бензилового эфира 2,2димеТил-циклопропанкарбоновой кислоты , а также растворитель - ацетон или диметилформамид и эмульгатор алкиларилполигликолевый эфир, отличающееся тем, что, с целью повышения инсектицидной активности , оно содержит в качестве производного бензилового эфира 2,2диметил-циклопропанкарбоновой кислаты соединение формулы НзС снз ClzFC СОгК С1 где R - пентафторбензил или группа формулы где R- водород или фтор; СО а в качестве алкиларилполигликолевого эфира - нонилфеноллолигликблевый эфир, при следующем соотношении компонентов , мас.%: Активный ингредиент 20 Растворитель 60 Эмульгатор 20 ...

VERFAHREN ZUR HERSTELLUNG VON CHLORCARBONSAEURECHLORIDEN

2,2-DIFLUORCYCLOPROPYL-DERIVATE.

Verfahren zur Herstellung von Carbonsäurechloriden

Herstellung von Fluorverbindungen aus Fluorsulfinaten der Alkalimetalle und quartaerer Stickstoffbasen

PROCESS FOR THE PREPARATION OF HALOGENATED ALIPHATIC CARBOXYLIC-ACID FLUORIDES

Plastische Massen zur Herstellung strahlungsundurchlaessiger Formkoerper

Verfahren zum Halogen-Fluor-Austausch in organischen Verbindungen und Katalysatoren hierzu.

PROCESS FOR THE PRODUCTION OF AROMATIC CARBOXYLIC-ACID CHLORIDES

ISOINDOLINYL-ALKYL-PIPERAZINVERBINDUNGEN, VERFAHREN ZU IHRER HERSTELLUNG UND PHARMAZEUTISCHE MITTEL

Production of chloroalkanoyl chloride, such as 5-chlorovaleryl chloride, used in synthesis of active pharmaceutical and agrochemical compounds, comprises introducing hydrogen chloride during heat-up in catalytic phosgenation of lactone

In the production of chloroalkanoyl chlorides (I) with a (substituted) 1-10 carbon (hetero)alkylene chain by reacting a lactone (II) with hydrogen chloride (HCl) and phosgene (COCl2) in the presence of a catalyst, HCl is introduced before and/or during addition of COCl2, starting when the temperature reaches >= 60 deg C, and the catalyst is a pyridine compound. In the production of chloroalkanoyl chlorides of formula (I) with a (substituted) 1-10 carbon (hetero)alkylene chain by reacting a lactone of formula (II) with hydrogen chloride (HCl) and phosgene (COCl2) in the presence of a catalyst, HCl is introduced before and/or during addition of COCl2, starting when the temperature reaches >= 60 deg C, and the catalyst is a pyridine compound: R<1>, R<2> = H or R; R = halogen, nitro, CN or an organic group containing carbon (C); Y = optionally R-substituted 1-10 C alkylene, which may have a (thio)ether, tertiary amino or keto group in the chain, in which R groups on Y, R<1> and/or R<2> may ...

Manufacture of octahydrophenanthrene-2-carboxylic acids and esters thereof

Sterically homogeneous octahydrophenanthrene-2-carboxylic acids and esters are manufactured by reacting a sterically homogeneous 1-keto-octahydrophenanthrene, containing in the 2-position a hydrocarbon radical and an esterified carboxyl group and in the 7-position a phenolic hydroxy group or a substituent convertible thereto, with an organo-metallic compound in order to introduce a hydrocarbon radical into the 1-position, directly or indirectly eliminating the resulting tertiary hydroxy group, separating the two isomers so obtained by fractional crystallization, chromatography or sublimation, and, if desired, converting the esterified carboxyl group in the 2-position into a free carboxyl group, or the substituent in the 7-position into a free hydroxy group, or both, in either order, and hydrogenating non-aromatic carbon-to-carbon multiple bonds at any desired stage after reaction with the organo-metallic compound. The starting material may be an individual racemate (obtainable by fractional ...

Improvements in the preparation of carboxylic acid chlorides

The invention comprises a process for preparing carboxylic chlorides by heating at 100 DEG to 375 DEG C. a mixture of carbon tetrachloride, a carboxylic acid, a carbocyclic or heterocyclic compound free from COOH groups and having at least one H on the aromatic nucleus, and a catalyst containing one or more oxides or mixed oxides of Mo, W, Si or Al or which is a metal salt of H2MoO2 or 3 or H2WO2 or 3, preferably in a mol. ratio of 2 : 1 : 1 of the reactants above. In examples, benzene, CCl4, acetic acid and a catalyst of reduced tungstic oxide react to give benzoyl and acetyl chlorides, with some terephthaloyl chloride, and isophthaloyl chloride; or with different proportions of reactants, benzoyl chloride; copper tungstite may also be used as catalyst; benzene, benzoic acid, CCl4 and reduced tungstic oxide give benzoyl chloride, terephthaloyl and isophthaloyl chlorides, products also obtained from benzene, terephthalic acid and CCl4; benzene, CO2 and CCl4 give COCl2 and benzoyl chloride ...

Improvements in the manufacture and production of halogenated hydrocarbon products, and analogous substances

... 301,009. Johnson, J. Y., (I. G. Farbenindustrie Akt.-Ges.). June 18, 1927. Divided on 301,000. Right to Patent relinquished. Halogenated hydrocarbons, halogenhydrins, nitriles, isonitriles, or halogenated acid chlorides are obtained from the products of destructive hydrogenation of carbonaceous materials by adding on halogens, hydrogen halides, hypohalogenous acids, hydrocyanic acid, or phosgene respectively to the double bonds. The destructive hydrogenation products may be subjected to a preliminary dehydrogenating, splitting, or cracking treatment of the kind referred to in Specification 298,584. In the addition of halogens or halogen halides, catalysts such as active charcoal, metal halides, iron oxide, or aluminium, or halogen transferrers such as phosphorus or iodine may be used. Hypochlorous acid may be added by the simultaneous action of a hypochlorite and carbon dioxide or of chlorine and water.

Manufacture of acetyl chloride

Acetyl chloride is prepared by treating vaporized acetic acid with phosgene (or with equal volumes of carbon monoxide and chlorine) in the presence of highly active carbon such as that obtained as described in Specifications 200,839 or 201,163, [both in Class 90, Non-metallic elements]. Details are given of tests whereby the suitability of an active carbon for use in the process may be ascertained. The active carbon may be used alone or mixed with silicic acid or a metal oxide, e.g. copper oxide, or a difficultly volatilizable metal chloride, e.g. cuprous or barium chloride. The reaction may be effected at reduced or raised pressure, but preferably at atmospheric pressure and a temperature of 200--250 DEG C. A small excess of acetic acid is preferably used. Specification 216,761, [Class 90, Non-metallic elements], also is referred to.

Improvements in the manufacture of acetyl-chloride

Acetyl chloride is prepared by the interaction of liquid acetic acid and gaseous phosgene at a raised temperature and approximately normal pressure under conditions whereby the acetyl chloride produced is continuously removed by evaporation. As catalysts for the reaction, use may be made of such compounds of metals of the second and third periodic groups as are soluble in hot acetic acid, e.g. magnesium oxide, anhydrous calcium chloride, or aluminium acetate. Examples are given in which the reaction is effected at 80 or 110 DEG C. in a vessel connected to a condenser which returns any acetic anhydride formed to the vessel, the acetyl chloride and the gaseous reaction products passing from the condenser to a refrigerator, and fresh acetic acid being continuously run into the vessel; the phosgene may be passed in through a porous plate in the vessel, and the gaseous reaction products undergoing cooling may be washed with a liquid which absorbs acetyl chloride without absorbing much hydrogen ...

Improvements in and relating to the production of substituted benzoyl halides

... 308,231. Bangham, P. F., Thomas, J., and Scottish Dyes, Ltd. Nov. 18, 1927À Benzoyl halides; benzoylaminoanthraquinones. -Substituted benzoyl halides are made by causing a substituted benzotrihaiide to react with a correspondingly substituted benzoic acid by means of an acidic metallic chloride, such as zinc chloride, in the absence of a solvent. The substituted benzotrihalide may be formed by halogenating the corresponding substituted toluene, and it may be converted into the substituted benzoic acid by treating with boiling milk of lime. The products may be purified by fractional distillation, preferably under reduced pressure, and may be employed for the benzoylation of amino compounds, particularly aminoanthraquinones. In examples, (1) o-chlorbenzotrichloride, obtained by passing chlorine into boiling o-chlortoluene, is heated with o-chlorbenzoic acid and zinc chloride, and (2) a mixture of o- and pchlortoluenes, obtained by chlorinating toluene in the cold in presence of ferric chloride ...

Process for the preparation of chlorocarboxylic acid chloride

A process for the preparation of a chlorocarboxylic acid chloride in which, in a first stage, a chlorocarboxylic acid is reacted with acetic anhydride and the acetic acid produced by the reaction is removed, and then the product obtained in the first stage is reacted with hydrogen chloride, in the absence of water, in a second reaction stage.

4-substituted-2-indanols

Alcohols of the formula in which R<1> is phenyl, optionally substituted with halogen or C1-4 alkyl are novel. They can be used in preparing insecticides of the pyrethroid type.

Chemical process

Chemical process

Improvements in or relating to dimethyl 2,3,5,6-tetrachloroterephthalate

Dimethyl 2, 3, 5, 6-tetrachloroterephthalate is prepared by reacting the molten acid chloride with an alkali and methanol. The 2, 3, 5, 6-tetrachlorotetraphthalyl chloride may be prepared by fusing together alpha, alpha-hexachloro-p-xylene and terephthalic acid and directly chlorinating the terephthalyl chloride so formed. Metal chloride catalysts, e.g. FeCl3, may be used for both the fusion and chlorination steps.

New indane-acetic acid aminoesters and their use in therapy

Compounds of the formula: (I) in which R represents an ethyl or isopropyl group, and their addition salts with acids or quaternary ammonium salts can be prepared from the compounds: in which R has the same meaning as above, and are valuable as analgesics.

Manufacture of organic acid halides and of derivatives therefrom

Organic acid halides are prepared by treating the acid with a carbon oxyhalide in the presence of a quantity of a nitrogen base amounting at most to one equivalent proportion for each acid group. The carbon oxyhalide may be replaced by such equivalent compounds as perchloroformic acid methyl ester and hexachlorocarbonic acid dimethyl ester. The nitrogen base not only fixes the hydrogen halide produced, but is stated to act catalytically. Bases mentioned are ammonia, trimethylamine, diethylamine, tetramethylethylenediamine, piperazine, methylaniline, diethylaniline, benzylaniline, diphenylamine, cyclohexylamine, pyridines, quinolines, piperidine, pyrazolones, quaternary ammonium compounds and guanidines. Acids which may be treated comprise aliphatic acids, e.g. acetic, valeric, palmitic, stearic, acrylic, crotonic, oleic, brassidic, propiolic and p tetrolic acids, halogenated fatty acids, aminoacetic and aminopropionic acids, nitro-fatty acids, diazo-fatty acids, glycollic and lactic acids ...

FUNGICIDE INTERMEDIATES

AZETIDINONES AND CONDENSED AZETIDINONES

... 1292729 Azetidinones, fused azetidinones and intermediates therefor CIBA-GEIGY AG 5 Dec 1969 [11 Dec 1968 8 July 1969] 52470/70 Divided out of 1289850 Headings C2C and C2P Novel compounds I (including salts and isomers thereof) where R 1 is H or an alcohol residue, R0 2 is H or acyl, Ac#0, which is easily removable under acidic conditions, R 3 is an organic residue and 0 0 R 4 a hydrogen atom when R 2 is Ac, or R 3 and R 4 together signify a disubstituted carbon atom 0 0 when R 2 is H or Ac, and R 0 signifies a methyl residue having at least one H and being mono- or di-substituted by optionally substitutedhydrocarbon, -heterocyclic or -heterocyclicaliphatic residues, or by functional groups, are made by reacting compounds IIIa with carboxaldehydes, R 0 .CO.CHO or with a tautomer or reactive derivative, e.g. hydrate, thereof (R a , R b and R c signify optionally substituted hydrocarbon residues). Products can be acylated, deacylated, esterified and/or saponified to afford ...

METHOD OF PRODUCING CARBOXYLIC ACID BROMIDES

... 1,210,475. Carboxylic acid bromides. CHEMISCHE FABRIK KALK G.m.b.H. 1 Feb., 1968 [3 Feb., 1967], No. 5262/68. Heading C2C. Carboxylic acid bromides are produced by mixing a carboxylic acid, phosphorus tribromide and bromine in the molar ratio of 3: 1: 1, the phosphorus tribromide being mixed with the acid before addition of the bromine, and then reacting the mixture at a temperature of 0‹-100‹ C.

LAVANDULIC ACID NITRILE AND LAVANDULYL beta-beta-DIMETHYLACRYLATE

... 1,244,188. Perfumes. L. GIVAUDAN & CIE S.A. 20 Dec., 1968 [10 Jan., 1969], No. 5633/71. Divided out of 1,244,187. Heading A5B. [Also in Division C2] Perfume compositions comprise either or both of the novel compounds lavandulic acid nitrile and lavandulyl #,#-dimethylacrylate [see Division C2 for preparation] together with additional odorous materials. In an Example a scented composition contains lavandulic acid nitrile, citral, eugenol, linalool oxide, oil of sage, phenylethyl acetate, -ionone, ylang, ylang synth, anethole, 2,6,10-trimethyl-9-undecen-1- al, pepermint oil, amyl salicylate, red thymian oil, linalool, coumarin, lavender oil, Californian orange oil, linalyl acetate and phthalic acid dieteryl ester.

BENZISOTHIAZOLINES

SUBSTITUTED AMIDES OF 3-METHYL-4-PHENYL-3-BUTENOIC ACID

... 1475644 3 - Methyl - 4 - phenyl - 3 - butenoic acid amides and their pharmaceutical compositions ISTITUTO BIOCHIMICO ITALIANO DI LOREDANA LORENZINI SAS 10 June 1975 [10 June 1974] 24826/75 Heading C2C The invention comprises amides of the general Formula III wherein R is hydrogen, C 1-6 alkyl, C 1-6 hydroxyalkyl or C 1-6 cycloalkyl and R1 is C 1-6 alkyl, C 1-6 hydroxy alkyl or C 1-6 cycloalkyl or wherein R and R1 together with the nitrogen atom to which they are attached form a morpholino ring which may be prepared by reaction of the acid chloride or a mixed anhydride of 3-methyl- 4-phenyl-3-butenoic acid with an amine of formula In exemplified compounds the amine is ethanolamine, diethanolamine, diethylamine, morpholine or cyclohexylamine. 3 - Methyl - 4 - phenyl - 3 - butenoylchloride is prepared by reaction of the parent acid with thionyl chloride. Pharmaceutical compositions having hypolipemizing activity comprise one or more compounds of Formula III together with ...

Process for the preparation of derived from hydrazine substituted.

Composed derived from the acid cyclohexylcarboxylic and their process of preparation.

Composed weedkillers, compositions the container and their processes of uses

New derivatives of the dibenzo [has, D] cycloheptene, their salts and their preparation.

Method of preparation of new acylamino acid.

STABILISIERTE ZUSAMMENSETZUNG

PROCEDURES FOR HERSETLLUNG OF P-HYDROXYPHENYLGLYCYLCHLORID, OF ITS HYDROCHLORIDE AND SOLVATEN

PROCEDURE FOR THE PRODUCTION OF FLUORINE COMPOUNDS OF MEANS LIQUID PHASE FLUORIDATION

VERFAHREN ZUR HERSTELLUNG NEUER, HALOGENIERTER BUTTERSAEURECHLORIDE

VERFAHREN ZUR HERSTELLUNG VON NEUEN 7-ACYLAMINOCEPHALOSPORINDERIVATEN

INSEKTIZIDE, AKARIZIDE UND NEMATOZIDE MISCHUNGEN

NEW PROCEDURE FOR THE PRODUCTION OF SÄURECHLORIDEN

PROCEDURE FOR the PRODUCTION OF NEW ONE 3,5-DIAMINO-6 (SUBSTITUTED PHENYL) - 1,2,4-TRIAZINEN AND THEIR ACID ADDITION SALTS

CHIRALES NEMATI LIQUID CRYSTAL MIXTURE

PROCEDURE FOR the PRODUCTION OF 2 (3-BENZOYL PHENYL) - PROPIONSAEURE

DIFLUORALKYLAROMATEN

PROCEDURE FOR ACYLATION OR ALKYLATION OF AROMATIC CONNECTIONS IN HYDROGEN FLUORIDES

PROCEDURE FOR THE PRODUCTION OF OPTICALLY ACTIVE ONES OR RACEMI CYCLOPROPANCARBONSÄURECHLORIDEN.

KOSMETIK AND EMULSIFYING COMPOSITION.

PROCEDURE FOR THE PRODUCTION OF NUCLEARFLUORIDATED BENZOIC ACID DERIVATIVES.

PROCEDURE FOR the PRODUCTION OF 5-PERFLUORALKYL-5,6-DIHYDROURACYL-DERIVATEN AND USABLE ONE INTERMEDIATE PRODUCTS.

PROCEDURE AND INTERMEDIATE CONNECTIONS FUER n (S-3ALKYL-HEPTANOYL) - D-GAMMA-GLUTAMYL-GLYCyl-DALANINE ONES.

FLUORINE-ALKENYL-SUBSTITUTED CYCLOPROPANCARBONSAEUREESTER (I), PROCEDURE FOR YOUR PRODUCTION, HERE RECEIVED INTERMEDIATE PRODUCTS AND THEIR PRODUCTION, the ESTERS (I) CONTAINING MEANS AND the USE of the ESTERS (I) FOR the FIGHT AGAINST INSECTS AND/OR ARACHNIDS.

MONOHYDROXY BENZOYL PEROXIDES AND COMPOSITIONS FOR THE TREATMENT OF ACNE.

PROCEDURE FOR THE PRODUCTION OF CYCLOPROPANCARBONSÄURE AND THEIR DERIVATIVES

PROCEDURE FOR THE PRODUCTION OF CHLORINE CARBONIC ACID CHLORIDE

Herbicide, in particular selectively herbicide, means

Procedure for the production of Oligomeren

COLORING MATERIAL-STABILIZED COMPOSITIONS

PROCEDURE FOR THE PRODUCTION OF THE NEW DL-TRANS-3,3-DIMETHYL-2-CYCLOPROPYLIDENMETHYL-1-CYCLOPROPANCARBONSAEURE AND THE NEW DL-TRANS-3,3-DIMETHYL-2-CYCLOBUTYLIDENMETHYL-1-CYCLOPROPANCARBONSAEURE AS WELL AS OF OF THEM DL-ALLETHROLONESTERN

Procedure for the production of new Pyrrolderivaten and their salts

METHYLENEALKANAMIDE COMPOUNDS

PROSTANOIC AND PROSTENOIC ACID DERIVATIVES AND INTERMEDIATES

Stereoselective synthesis of A 4,4-disubstituted cyclohexanepropanoic acid

Matrix metalloprotease inhibitors________________________________

Malonic acid di-salts and a method for preparing malonyl dihalides

A compound of Formula (2) is disclosed: wherein R ...

((2-OXEPANYLIDENE)METHYL)TRIPHENYL PHOSPHONIUM COMPOUNDS

FLUOROALKENYL-SUBSTITUTED CYCLOPROPANECARBOXYLIC ACID ESTER

INDOLIZINO 8,7BETA INDOLE DERIVATIVES

PROCESS FOR PREPARING N-PHOSPHONO-METHYL-IMINO-DIACETIC ACID AND ACID CHLORIDE

PHARMACEUTICALLY ACTIVE CYCLOHEXYL COMPOUNDS AND THEIR PREPARATION

METHOD FOR THE PRODUCTION OF BENZOPHENONES

Disclosed is a method for producing benzophenones of formula I, wherein X can represent chlorine, hydroxy, methoxy, or C1-C6 alkylcarbonyloxy while Y represents chlorine or bromine, by reacting an acid chloride of formula II, wherein X and Y have the meaning mentioned above, with 3,4,5- trimethoxytoluene. The inventive method is characterized by the fact that the reaction is carried out in the presence of a) an aromatic hydrocarbon as a thinner, and b) 0.01 to 0.2 mole percent of an iron catalyst, the percentage being in relation to the acid chloride, c) at a temperature ranging between 60oC and the boiling point of the respective thinner.

PROCESS FOR CARBOXYLIC ACID HALIDE MANUFACTURE

PROCESS FOR THE PREPARATION OF HALOGENATED ALIPHATIC CARBOXYLIC ACID FLUORIDES

... of the disclosure: Halogenated aliphatic carboxylic acid fluorides are prepared by reacting halogenated aliphatic carboxylic acids with trihalogenomethyl aromatic compounds containing, as a predominant total or exclusively, fluorine atoms in the trihalogenomethyl groups, in particular with benzotrifluoride, in the presence of Lewis acids as catalysts. The reaction products are intermediate products having a multiplicity of uses.

PERFLUOROALKYLACETYL CHLORIDES AND PROCESS FOR THEIR MANUFACTURE

HOE 75/F 927 K PERFLUOROALKYLACETYL CHLORIDES AND PROCESS FOR THEIR MANU FACTURE . Perfluoroalkylacetyl chlorides of the formula I. wherein Rf represents a straight-chain perfluoro alkyl radical having from 4 to 12 carbon atoms which are prepared by reacting perfluoro alkyl ethanols having general formula Rf . CH2 . CH2 . OH II. wherein Rf has the same meaning as in formula I, with chlorine under exposure to UV radiation, in the presence of an inert organic solvent, at temperatures of from -20.degree.C to +120.degree.C. These acetyl chlorides are intermediates for the preparation of the corresponding esters with polyglycols which serve as dry cleaning detergents.

BRANCHED FATTY ACID CHOLESTEROL ESTER AND A COSMETIC COMPOSITION CONTAINING THE SAME

A branched fatty acid cholesterol ester represented by the formula (I): (I) where, R is a saturated aliphatic hydrocarbon group having a total of 11 to 23 carbon atoms and including at least one alkyl substituent group attached on the main chain inbetween the carboxyl bonding position and the center of the main chain; and cosmetic compositions containing the same are disclosed.

PREPARATION OF MONO- AND DIBROMO- OR CHLOROALDEHYDES AND ACID CHLORIDES

A process for making mono- and dichlorinated or brominated aldehydes and acid chlorides from aldehydes having hydrogens alpha to the carbonyl group or primary alcohols having hydrogens in the 2-position by direct bromination or chlorination by carrying out the bromination or chlorination in an inert organic solvent saturated with bromine or chlorine and containing a catalyst complex of hydrogen chloride and an N,N-dialkyl or cycloalkylformamide.

INTERFACIAL PRODUCTION OF POLY(ESTER CARBONATE) OR POLYESTER INCLUDING ACID CHLORIDE SYNTHESIS

An alkali metal or alkaline earth metal salt of an aromatic or cycloaliphatic dicarboxylic acid such as the disodium or dipotassium salt of terephthalic or isophthalic acid is reacted with phosgene in an inert organic solvent in the presence of a tertiary nitrogen compound such as pyridine. The solid alkali metal or alkaline earth metal chloride salts which are by-products are easily separated from the organic solution containing the product acid chloride. The solution is then, in some form, interfacially reacted with a bisphenol such as bisphenol A. Excess phosgene in the diacid chloride synthesis can be carried over to the polymerization if a poly(ester carbonate) is to be produced or removed if a polyester is to be produced. Certain low levels of a tertiary nitrogen compound with a pyridine nucleus in the organic solution do not interfere with the interfacial polymerization.

N-(MERCAPTOACYL) AMINOACIDS

PREPARATION OF ACYL CHLORIDES

... where R is C8-C30-alkyl, C8-C30-alkenyl or C8-C30-alkynyl, from a carboxylic acid of the general formula II where R has the abovementioned meanings, and phosgene, COC1 2 (III), in the presence of a catalyst adduct of phosgene and N,N-dialkylformamide of the general formula IV where R1 and R2 independently of one another are each C1-C3-alkyl, the reaction product I being obtained by phase separation, by a process in which II and III are used in essentially equimolar amounts and the phase containing the catalyst adduct is reused.

METHOD FOR PRODUCING O-CHLOROMETHYL BENZOIC ACID CHLORIDES

The invention relates to a method for producing o-chloromethyl benzoic acid chlorides of formula (I), in which R1 to R4 can be the same or different and represent hydrogen C1-C4 alkyl, halogen or trifluoromethyl, by reacting benzo- condensed lactones of formula (II), in which R1 to R4 have the above-mentioned meaning, with thionyl chloride. The inventive method is characterized in that the reaction is carried out in the presence of catalytic quantities of a Lewis acid and in the presence of catalytic quantities of a phosphine derivative.

LENHANCEMENT OF FLAVOR IN FOODSTUFFS

PROCESS FOR THE PREPARATION OF OXALYL CHLORIDE

3,5-BISOXYGENATED 2-((OMEGA)-HALO-3-OXYGENATED-1- ALKENYL)CYCLOPENTANE-1-HEPTANOIC ACIDS AND DERIVATIVES THEREOF

A METHOD FOR PREPARING FATTY ACID CHLORIDES

A method is disclosed for preparing fatty acid chlorides and comprises reacting a silylation product of a fatty acid comprising at least 2 aliphatically unsaturated bonds per molecule and a chlorinating agent.

Verfahren zum Wasser- und Ölabweisendmachen von Textilien

VERFAHREN ZUR HERSTELLUNG VON PARTIELL HYDRIERTEN RINGSUBSTITUIERTEN PHENANTHREN-2-CARBONSAEUREN.

Verfahren zur Herstellung eines Carbonsäurechloridgemisches.

Verfahren zur Herstellung eines Carbonsäurechloridgemisches.

Verfahren zum Wasser- und Ölabweisendmachen von Textilien

Accelerator Mixture for Peroxide Hardener and Two-Component Mortar System Containing Same

An accelerator mixture for peroxide hardeners, in particular an accelerator mixture for an organic peroxide-curing resin mixture, a two-component mortar system containing the same for chemical fastening and use of the same for chemical fastening of anchoring elements in boreholes are disclosed. Using a mixture of bis-N-substituted p-toluidines with bis-N-substituted anilines or bis-N-substituted m-toluidines, it is possible to provide a mortar composition for chemical fastening of anchoring elements in boreholes, which will have an improved low-temperature curing and improved load ratings at high temperatures with an extended gel time. 2. The accelerator mixture according to claim 1 , wherein the main accelerator (I) is N claim 1 ,N-bis(2-hydroxyethyl)-p-toluidine claim 1 , N claim 1 ,N-bis(2-hydroxypropyl)-p-toluidine or an ethoxylated or propoxylated derivative thereof.3. The accelerator mixture according to claim 1 , wherein the co-accelerator (II) is N claim 1 ,N-diethylaniline claim 1 , N claim 1 ,N-bis(2-hydroxyethyl)aniline claim 1 , N-ethyl-N-hydroxyethylaniline claim 1 , N claim 1 ,N-bis(2-hydroxyethyl)-m-toluidine or N claim 1 ,N-bis(2-hydroxypropyl)-m-toluidine.4. The accelerator mixture according to claim 3 , wherein the main accelerator (I) is N claim 3 ,N-bis(2-hydroxypropyl)-p-toluidine and the co-accelerator (II) is N claim 3 ,N-bis(2-hydroxyethyl)-m-toluidine.5. The accelerator mixture according to claim 1 , wherein a molar ratio of the main accelerator (I) to the co-accelerator (II) is 3:1.6. A resin mixture claim 1 , comprising:a radically polymerizable compound;{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, 'an accelerator according to ; and'}optionally an inhibitor and a reactive diluent.7. The resin mixture according to claim 6 , wherein the main accelerator (I) is N claim 6 ,N-bis(2-hydroxypropyl)-p-toluidine and the co-accelerator (II) is N claim 6 ,N-bis(2-hydroxyethyl)-m-toluidine.8. The resin mixture according to claim 6 , wherein a ...

PROCESS FOR THE SELECTIVE OXIDATION OF CARBON MONOXIDE

The invention relates to a process of the selective oxidation of carbon monoxide to carbon dioxide present in a gas mixture comprising at least one hydrocarbon or a hydrocarbon derivative, and to its integration into a process for producing hydrocarbon derivatives. The process according to the invention comprises a step that consists in bringing said gas mixture into contact with a solid catalyst capable of oxidizing carbon monoxide to carbon dioxide at a chosen temperature, characterized on that said step is carried out in a fluidized bed. 1. A process for the selective oxidation of carbon monoxide present in a gas mixture comprising at least one hydrocarbon or one hydrocarbon derivative and carbon monoxide , said process comprising bringing said gas mixture into contact with a fluidized bed of a solid oxidizing catalyst whereby said carbon monoxide is oxidized to carbon dioxide at a chosen temperature.2. The process as claimed in claim 1 , characterized in that the hydrocarbon is a saturated or mono- or diunsaturated linear or branched hydrocarbon comprising from 2 to 6 carbon atoms claim 1 , or an aromatic hydrocarbon comprising from 6 to 12 carbon atoms.3. The process as claimed in claim 1 , characterized in that the hydrocarbon derivative is selected from the group consisting of anhydrides claim 1 , aldehydes claim 1 , unsaturated carboxylic acids claim 1 , unsaturated nitriles claim 1 , mixtures thereof claim 1 , ethylene oxide claim 1 , propylene oxide and 1 claim 1 ,2-dichloroethane.4. The process as claimed in claim 1 , characterized in that the catalyst is in the form of solid particles with a particle size ranging from 20 to 1000 microns.5. The process as claimed in claim 1 , characterized in that the catalyst is selected from the group consisting of catalysts based on noble metals supported on an inorganic support.6. The process as claimed in claim 1 , characterized in that the temperature of the fluidized bed is lower than the temperature corresponding ...

Electrochemical Co-Production of Chemicals Employing the Recycling of a Hydrogen Halide

The present disclosure is a system and method for producing a first product from a first region of an electrochemical cell having a cathode and a second product from a second region of the electrochemical cell having an anode. The method may include a step of contacting the first region with a catholyte comprising carbon dioxide. The method may include another step of contacting the second region with an anolyte comprising a recycled reactant. The method may include a step of applying an electrical potential between the anode and the cathode sufficient to produce a first product recoverable from the first region and a second product recoverable from the second region. The second product may be removed from the second region and introduced to a secondary reactor. The method may include forming the recycled reactant in the secondary reactor. 1. A method for producing a first product from a first region of an electrochemical cell having a cathode and a second product from a second region of the electrochemical cell having an anode , the method comprising the steps of:contacting the first region with a catholyte comprising carbon dioxide;contacting the second region with an anolyte comprising a recycled reactant;applying an electrical potential between the anode and the cathode sufficient to produce a first product recoverable from the first region and a second product recoverable from the second region;removing the second product from the second region;introducing the second product to a secondary reactor; andforming the recycled reactant in the secondary reactor.2. The method according to claim 1 , wherein the recycled reactant is a hydrogen halide claim 1 , HX claim 1 , where X is selected from a group consisting of F claim 1 , Cl claim 1 , Br claim 1 , I claim 1 , and mixtures thereof.3. The method according to claim 2 , wherein the second product is X.4. The method according to claim 3 , wherein the reaction in the secondary reactor includes an alkane claim 3 , ...

PROCESS FOR THE PREPARATION OF INTERMEDIATES FOR THE MANUFACTURE OF NEP INHIBITORS

The invention relates to a new process for producing useful intermediates for the manufacture of NEP inhibitors or prodrugs thereof, in particular NEP inhibitors comprising a γ-amino-δ-biphenyl-α-methylalkanoic acid, or acid ester, backbone, such as N-(3-carboxyl-1-oxopropyl)-(4S)-(p-phenylphenylmethyl)-4-amino-(2R)-methyl butanoic acid ethyl ester or salt thereof. 2. A process according to wherein the transition metal catalyst comprises Palladium (Pd).3. A process according to wherein the transition metal catalyst is Pd(PPh).4. A process according to whereinR1 is hydrogen;R2 is BOC; andR3 is a carboxyl group.5. A process for preparing N-(3-carboxyl-1-oxopropyl)-(4S)-(p-phenylphenylmethyl)-4-amino-(2R)-methyl butanoic acid ethyl ester claim 1 , or a salt thereof claim 1 , comprising the manufacture of compound of formula (3) claim 1 , or salt thereof claim 1 , as defined in .6. A process for preparing N-(3-carboxyl-1-oxopropyl)-(4S)-(p-phenylphenylmethyl)-4-amino-(2R)-methyl butanoic acid claim 1 , or a salt thereof claim 1 , or a prodrug thereof claim 1 , comprising the manufacture of compound of formula (3) claim 1 , or salt thereof claim 1 , as defined in . The invention relates to a new process for producing useful intermediates for the manufacture of NEP inhibitors or prodrugs thereof, in particular NEP inhibitors comprising a γ-amino-δ-biphenyl-α-methylalkanoic acid, or acid ester, backbone.Endogenous atrial natriuretic peptides (ANP), also called atrial natriuretic factors (ANF) have diuretic, natriuretic and vasorelaxant functions in mammals. The natural ANF peptides are metabolically inactivated, in particular by a degrading enzyme which has been recognized to correspond to the enzyme neutral endopeptidase (NEP, EC 3.4.24.11), also responsible for e.g. the metabolic inactivation of enkephalins.In the art biaryl substituted phosphonic acid derivatives are known which are useful as neutral endopeptidase (NEP) inhibitors, e.g. as inhibitors of the ANF- ...

PROCESS FOR PREPARATION OF RUFINAMIDE

The invention relates to a novel, industrially viable, cost effective process for the preparation of 1-(2,6-difluorobenzyl)-1H-1,2,3-triazole-4-carboxamide commonly known as Rufinamide and intermediates thereof. 2. The process according to claim 1 , wherein R is hydrogen claim 1 , methyl or ethyl.3. The process according to claim 1 , wherein formula V is selected from 2-bromoacrylic acid claim 1 , methyl 2-bromoacrylate and ethyl 2-bromo acrylate.4. The process according to claim 1 , wherein the compound of formula VI prepared in step (b) is methyl 1-(2 claim 1 ,6-difluorobenzyI)-1H-1 claim 1 ,2 claim 1 ,3-triazole-4-carboxylate.6. The process according to claim 5 , wherein the compound of formula V is selected from 2-bromoacrylic acid claim 5 , methyl 2-bromoacrylate and ethyl 2-bromo acrylate.7. The process according to claim 5 , wherein the compound prepared is methyl 1-(2 claim 5 ,6-difluorobenzyl)-1H-1 claim 5 ,2 claim 5 ,3-triazole-4-carboxylate.9. The process according to claim 8 , wherein R is hydrogen claim 8 , methyl or ethyl.10. The process according to claim 9 , wherein R is methyl.11. The process according to claim 8 , wherein the brominating agent is selected from the group consisting of phosphorus tribromide claim 8 , aluminum tribromide and bromine.12. The process according to claim 11 , wherein the brominating agent is bromine.13. The process according to claim 8 , wherein the base is selected from the group consisting of sodium carbonate claim 8 , sodium bicarbonate claim 8 , potassium carbonate claim 8 , potassium bicarbonate claim 8 , potassium t-butoxide and triethylamine.14. The process according to claim 13 , wherein sodium carbonate and triethylamine is used as base.15. The process according to claim 8 , wherein the compound prepared is methyl 2-bromoacrylate. The invention provides a novel, industrially viable, cost effective process for manufacturing methyl 1-(2,6-difluorobenzyl)-1H-1,2,3-triazole-4-carboxylate a key intermediate in the ...

Novel Intermediate for Preparing Tapentadol or Analogues Thereof

The invention discloses a novel intermediate for preparing tapentadol and analogues thereof, wherein the structural formula is shown as formula I or II, and the groups are defined as the specification. The invention further discloses a method for preparing the novel intermediate and use of the intermediate for preparing tapentadol and analogues thereof. The invention can remarkably improve the product yield and quality of tapentadol, reduce the production cost, and simplify the production procedure. The preparation process is environment friendly, thus more suitable for the requirements of industrial production. 2. The compound according to claim 1 , wherein Ris selected from Cl claim 1 , methyl claim 1 , OH claim 1 , NHor methoxy.3. The compound according to claim 1 , characterized in that Y is selected from OR claim 1 , wherein Ris selected from methyl claim 1 , ethyl claim 1 , n-propyl or isopropyl.4. The compound according to claim 1 , characterized in that Y is selected from NRR claim 1 , wherein R claim 1 , Rand N form substituted or unsubstituted saturated nitrogen-containing heteorcyclyl containing oxygen or not jointly.5. The compound according to claim 4 , wherein R claim 4 , Rand N form tetrahydropyrrole ring claim 4 , piperidine ring claim 4 , 4-methylpiperidine ring claim 4 , morpholine ring claim 4 , methylpiperazine ring or 4-hydroxypiperidine jointly.6. The compound according to claim 1 , selected from the following compounds:valeryl 2-methyl-3-(3-methoxyphenyl)chloride;methyl 2-methyl-3-(3-methoxyphenyl)sulfovalerate;methyl 2-methyl-3-(3-hydroxyphenyl) ulfovalerate;2-methyl-3-(3-hydroxyphenyl)sulfovaleramide;N,N-dimethyl-2-methyl-3-(3-methoxyphenyl)sulfovaleramide;N,N-dimethyl-2-methyl-3-(3-hydroxyphenyl)sulfovaleramide;N,N-diethyl-2-methyl-3-(3-methoxyphenyl)valeramide;3-(3-methoxyphenyl)-2-methyl-1-(piperidin-1-yl)pentan-1-one;3-(3-methoxyphenyl)-2-methyl-1-(4-methylpiperidin-1-yl)pentan-1-one;3-(3-methoxyphenyl)-2-methyl-1-(morpholin-1-yl)pentan- ...

TWO ATOM BRIDGED DICARBONATE COMPOUNDS AS INTERNAL DONORS IN CATALYSTS FOR POLYPROPYLENE MANUFACTURE

A compound suitable for use as an internal electron donor having a structure: 2. The compound of wherein R1 is independently at each occurrence claim 1 , an aliphatic or aromatic hydrocarbon group containing from 1 to 6 carbon atoms; and R2 is independently at each occurrence claim 1 , a hydrogen atom or aliphatic or aromatic hydrocarbon group containing from 1 to 6 carbon atoms; and R3 is an aliphatic hydrocarbyl group having 1 to 3 carbon atoms.3. The compound of wherein R1 is independently at each occurrence claim 1 , a methyl claim 1 , ethyl claim 1 , isopropyl claim 1 , t-butyl claim 1 , or phenyl group; and R2 is independently at each occurrence claim 1 , a hydrogen atom or a methyl claim 1 , ethyl claim 1 , or isopropyl group; and R3 is a methyl claim 1 , ethyl claim 1 , or isopropyl group.4. The compound of wherein R1 is independently at each occurrence claim 1 , an ethyl claim 1 , isopropyl claim 1 , t-butyl claim 1 , or phenyl group; and R2 is independently at each occurrence claim 1 , a hydrogen atom; and R3 is a methyl or isopropyl group. This application is a non-provisional application claiming priority from the U.S. Provisional Patent Application No. 61/265,931, filed on Dec. 2, 2009, and also from the U.S. National Utility application Ser. No. 12/956,050, filed on Nov. 30, 2010, entitled “TWO ATOM BRIDGED DICARBONATE COMPOUNDS AS INTERNAL DONORS IN CATALYSTS FOR POLYPROPYLENE MANUFACTURE,” the teachings of which are incorporated by reference herein, as if reproduced in full hereinbelow.This invention relates to components useful in propylene polymerization catalysts, and particularly relates to electron donor components used in combination with magnesium-containing supported titanium-containing catalyst components.Use of solid, transition metal-based, olefin polymerization catalyst components is well known in the art including such solid components supported on a metal oxide, halide or other salt such as widely-described magnesium-containing, ...

METAL CARBAMATES FORMED FROM DIAMINOPHENYLMETHANE

The invention provides metal carbamates of the general formula (I) 1. (canceled)3. The process of claim 2 , wherein claim 2 , in formula (I) claim 2 , the alkyl groups Rand Reach comprise 2-18 carbon atoms in the chain.4. The process of claim 2 , wherein claim 2 , in formula (I) claim 2 , the alkyl groups Rand Reach comprise 2-7 carbon atoms in the chain.5. The process of claim 2 , wherein claim 2 , in formula (I) claim 2 , the alkyl groups Rand Rare each independently an ethyl claim 2 , propyl claim 2 , butyl claim 2 , 2-methylpropyl claim 2 , 3-methylbutyl claim 2 , n-pentyl claim 2 , 2-methoxyethyl claim 2 , 2-ethoxyethyl claim 2 , or a 2 claim 2 ,2 claim 2 ,2-trifluoroethyl group.6. The process of claim 2 , wherein claim 2 , in formula (I) claim 2 , the alkyl groups Rand Rcomprise heteroatoms.7. The process of claim 6 , wherein the heteroatoms are halogen atoms.8. The process of claim 6 , wherein the heteroatoms are fluorine atoms.9. The process of claim 6 , wherein the heteroatoms are chlorine atoms.10. The process of claim 6 , wherein the heteroatoms are oxygen atoms.11. The process of claim 6 , wherein the heteroatoms are oxygen atoms present in the form of ether groups.12. The process of claim 2 , wherein claim 2 , in formula (I) claim 2 , the alkali metal ion is lithium.13. The process of claim 2 , wherein claim 2 , in formula (I) claim 2 , the alkali metal ion is sodium.14. The process of claim 2 , wherein claim 2 , in formula (I) claim 2 , the alkali metal ion is potassium.15. The process of claim 2 , wherein claim 2 , in formula (I) claim 2 , wherein Rand Rare identical.16. The process of claim 3 , wherein claim 3 , in formula (I) claim 3 , Rand Rare identical.17. The process of claim 4 , wherein claim 4 , in formula (I) claim 4 , Rand Rare identical.18. The process of claim 5 , wherein claim 5 , in formula (I) claim 5 , Rand Rare identical.19. The process of claim 6 , wherein claim 6 , in formula (I) claim 6 , Rand Rare identical. This application is a ...

PROCESS FOR PREPARING FORMIC ACID

A process for preparing formic acid by hydrogenation of carbon dioxide in the presence of a tertiary amine (I), a diamine (II), a polar solvent and a catalyst comprising gold at a pressure of from 0.2 to 30 MPa abs and a temperature of from 0 to 200° C., wherein the catalyst is a heterogeneous catalyst comprising gold. 115-. (canceled)16. A process for preparing formic acid by hydrogenation of carbon dioxide in the presence of a tertiary amine (I) , a diamine (II) , a polar solvent and a catalyst comprising gold at a pressure of from 0.2 to 30 MPa abs and a temperature of from 0 to 200° C. , wherein the catalyst is a heterogeneous catalyst comprising gold.17. The process of claim 16 , wherein the heterogeneous catalyst comprising gold is a supported catalyst.18. The process of claim 17 , wherein the supported heterogeneous catalyst comprises silicon dioxide claim 17 , aluminium oxide claim 17 , zirconium oxide claim 17 , magnesium oxide and/or titanium oxide as support.19. The process of claim 17 , wherein the supported heterogeneous catalyst comprises 0.1 to 20 wt.-% gold based on the total mass of the supported catalyst.20. The process of claim 16 , wherein the tertiary amine (I) comprises at least 12 carbon atoms.21. The process of claim 16 , wherein the tertiary amine (I) is tripentylamine claim 16 , trihexylamine and/or a triheptylamine.23. The process of claim 16 , wherein the diamine (II) is selected from the group consisting of N claim 16 ,N claim 16 ,N′ claim 16 ,N′-tetramethyl-ethane-1 claim 16 ,2-diamine (TMEDA) claim 16 , N claim 16 ,N claim 16 ,N′ claim 16 ,N′-tetramethyl-butane-1 claim 16 ,4-diamine claim 16 , pentamethylenedipiperidine (1 claim 16 ,1′-(1 claim 16 ,5-pentanediyl)bis-piperidine) claim 16 , tetramethylenedipyrrolidine (1 claim 16 ,1′-(1 claim 16 ,4-butanediyl)bis-pyrrolidine) claim 16 , 1 claim 16 ,8-diaza-bicylo[5.4.0]undec-7-ene (DBU) claim 16 , 1 claim 16 ,5-diazabicyclo[4.3.0]non-5-ene (DBN) claim 16 , bicyclo[2.2.2]-1 claim 16 ,4- ...

Method for Purifying Difluoroacetic Acid Chloride

A method for purifying difluoroacetic acid chloride, including the step of bringing a difluoroacetic acid chloride composition that contains at least difluoroacetic acid fluoride into contact with calcium chloride at a temperature enabling reaction thereof thereby converting difluoroacetic acid fluoride into difluoroacetic acid chloride. 1. A method for purifying difluoroacetic acid chloride , comprising the step of:bringing a difluoroacetic acid chloride composition that contains at least difluoroacetic acid fluoride into contact with calcium chloride at a temperature enabling reaction thereof thereby converting difluoroacetic acid fluoride into difluoroacetic acid chloride.2. A method for purifying difluoroacetic acid chloride claim 1 , as claimed in claim 1 , wherein the contact comprises the step of causing the difluoroacetic acid chloride composition to flow through calcium chloride at a temperature enabling reaction thereof.3. A method for purifying difluoroacetic acid chloride claim 1 , as claimed in claim 1 , wherein the reaction temperature is 50 to 250° C.4. A method for purifying difluoroacetic acid chloride claim 1 , as claimed in claim 1 , wherein the retention time is 1 to 1000 seconds.5. A method for purifying difluoroacetic acid chloride claim 1 , as claimed in claim 1 , wherein the reaction is conducted in a liquid phase.6. A method for purifying difluoroacetic acid chloride claim 1 , comprising the step of:reacting difluoroacetic acid fluoride with lithium chloride thereby producing a difluoroacetic acid chloride composition that contains at least difluoroacetic acid fluoride; andbringing the difluoroacetic acid chloride composition into contact with calcium chloride at a temperature enabling reaction thereof thereby converting difluoroacetic acid fluoride into difluoroacetic acid chloride.7. A method for purifying difluoroacetic acid chloride claim 6 , as claimed in claim 6 , wherein the contact comprises the step of causing the difluoroacetic ...

Process for the Production of 4-Chloroacetoacetyl Chloride, 4-Chloroacetoacetic Acid Esters, Amides and Imides

The invention relates to process for the continuous production of 4-chloroacetoacetyl chloride, comprising the steps of (a) feeding diketene and chlorine into a thin film reactor and (b) reacting the diketene and chlorine to obtain 4-chloroacetoacetyl chloride. The invention also relates to a process for the production of 4-chloroacetoaceticacid ester, 4-chloroacetoaceticacid amide or 4-chloroacetoaceticacid imide from 4-chloroacetoacetyl chloride obtained according to the inventive process. 114-. (canceled)16. The process of claim 15 , wherein the solvent is a halogenated alkane claim 15 , preferably selected from chloromethane claim 15 , dichloromethane claim 15 , trichloromethane (chloroform) claim 15 , tetrachloromethane claim 15 , chloroethane claim 15 , 1 claim 15 ,2-dichlorethane claim 15 , trichloroethane claim 15 , tetrachloroethane claim 15 , dichloropropane claim 15 , 1-chloro-2-fluoroethane claim 15 , 1 claim 15 ,1-dichloroethane claim 15 , 1 claim 15 ,2-dichloroethane claim 15 , methylchloroform claim 15 , 1-chlorobutane claim 15 , 2-chlorobutane claim 15 , 1-bromobutane claim 15 , ethyl bromide claim 15 , 1-bromo-2-chloroethane claim 15 , 1-bromo-2-fluoroethane claim 15 , 1-iodobutane claim 15 , bromochloromethane claim 15 , dibromomethane claim 15 , 1 claim 15 ,1-dibromomethane claim 15 , difluoroiodomethane claim 15 , 1-bromopropane claim 15 , bromochlorofluoromethane claim 15 , 2-bromopropane claim 15 , bromodichloromethane claim 15 , bromofluoromethane claim 15 , bromotrichloromethane claim 15 , dibromodifluoromethane claim 15 , pentachloromethane claim 15 , 1 claim 15 ,1 claim 15 ,1 claim 15 ,2-tetrachloroethane claim 15 , fluoroiodomethane claim 15 , iodomethane claim 15 , diiodofluoromethane claim 15 , 1 claim 15 ,1 claim 15 ,2 claim 15 ,2-tetrachloromethane claim 15 , 1 claim 15 ,1 claim 15 ,2-trichloroethane claim 15 , 1-chloropropane claim 15 , 1 claim 15 ,2-dibromopropane claim 15 , 1 claim 15 ,2 claim 15 ,3-trichloropropane claim 15 , 1 ...

METHOD FOR PRODUCING ACETYLENEDICARBOXYLIC ACID FROM ACETYLENE AND CARBON DIOXIDE

The invention relates to a method for producing acetylenedicarboxylic acid by reaction of acetylene with carbon dioxide, wherein the reaction is carried out in the presence of a silver or copper salt and an amine base. 1. A method for producing acetylenedicarboxylic acid by reaction of acetylene with carbon dioxide , wherein the reaction is carried out in the presence of a silver or copper catalyst and an amine base.2. The method according to wherein the silver catalyst is selected from the group consisting of silver(l) halides claim 1 , silver(l) nitrate and silver tetrafluoroborate.3. The method according to wherein the copper catalyst is chosen from the group consisting of copper(l) iodide and copper(l) cyanide.4. The method according to wherein the amine base is chosen from the group consisting of 1 claim 1 ,5-diazabicyclo[4.3.0]non-5-ene (DBN) and 1 claim 1 ,8-diazabicyclo[5.4.0]undec-7-ene (DBU).5. The method according to wherein the reaction is carried out in a solvent.6. The method according to wherein the reaction is carried out at a total pressure of 1-50 bar and a temperature of 50 to 120° C.7. The method according to wherein the reaction is carried out with a molar ratio of carbon dioxide to acetylene of 2:1 to 50:1. The invention relates to a method for producing acetylenedicarboxylic acid by reaction of acetylene with carbon dioxide.According to an historic method, dating back to the year 1877, acetylenedicarboxylic acid is formed from meso-dibromosuccinic acid by alkaline elimination.The formation of acetylenedicarboxylic acid with a yield of 34% by reacting dilithium carbide, obtained from reaction of vinyl bromide with butyllithium, with carbon dioxide in ether, where the carbon dioxide is added as dry ice, is described in E. C. Horning, J. Am Chem. Soc. 1945, 67, 1412-1422.Acetylenedicarboxylic acid may be obtained in a yield of ca. 50% by the electrochemical oxidation of alkynols at the anode with lead oxide electrodes. An electrochemical method ...

REACTIVE EXTRACTION PROCESS FOR REGENERATION OF AMINE-BASED SOLVENTS USED FOR CARBON DIOXIDE CAPTURE

A method for recovery of impurities and/or degradation products and/or heat-stable salts from amine-based solvents used for capture of C0from gas streams. The method comprises recovering C0from a C0-enriched amine-based solvent thereby producing a lean amine-based solvent, contacting and mixing together the lean amine-based solvent with a reaction composition comprising a phase-change catalyst and a diluent, thereby producing a first organic phase comprising the impurities and/or degradation products and/or heat-stable salts and a first aqueous phase comprising the lean amine-based solvent, separating the first organic phase and the first aqueous phase; and separately recovering the first organic phase and the first aqueous phase. The organic phase can be regenerated by intermixing with a NaOH solution to form an organic phase comprising therein the reaction composition and and an aqueous phase comprising the NaOH solution with the impurities and/or degradation products and/or heat-stable salts. 1. A one-stage method for recovery of impurities and/or degradation products and/or heat-stable salts from spent amine-based solvents used for capture of COfrom gas streams , the method comprising:{'sub': 2', '2, 'recovering COfrom a spent CO-enriched amine-based solvent thereby producing a lean amine-based solvent;'}contacting and mixing together the lean amine-based solvent with a reaction composition comprising a phase-change catalyst and a diluent, thereby producing a first organic phase comprising the impurities and/or degradation products and/or heat-stable salts and a first aqueous phase comprising a purified lean amine-based solvent;separating the first organic phase and the first aqueous phase; andseparately recovering the first organic phase and the first aqueous phase.2. The one-stage method of claim 1 , additionally comprising a step of recycling the purified lean amine-based solvent for capturing COfrom a gas stream.3. The one-stage method of claim 1 , ...

METHOD FOR PRODUCING DIARYL CARBONATE

The present application relates to a method for the continuous production of diaryl carbonate from phosgene and of at least one monohydroxy compound (monophenol) in the presence of catalysts, and to the use thereof for the production of polycarbonates. 111.-. (canceled)12. A process for preparing diaryl carbonate by reaction of an aromatic hydroxyl compound and a halogenated carbonyl in the presence of a catalyst in a reactor , wherein the ratio G/A is less than 0.010 , where G is the entry volume flow rate of the liquid or dissolved halogenated carbonyl in m/s and A is the internal cross-sectional area orthogonal to the longitudinal axis in m.13. The process as claimed in claim 12 , wherein the reaction takes place in a bubble column reactor in the absence of a solvent.14. The process as claimed in claim 12 , wherein G/A is in the range from 0.0005 [m/s] and 0.0095 [m/s].15. The process as claimed in claim 12 , wherein the ratio H/D is greater than or equal to 2 and H is the height of the liquid phase in the reactor in the gas-free state and D is the diameter of the reactor.16. The process as claimed in claim 12 , wherein the residence time in the reactor is in the range from 0.5 to 4 hours claim 12 , the temperature is in the range from 120 to 220° C. and the pressure is 3 to 100 bar.17. The process as claimed in claim 12 , wherein the halogenated carbonyl is phosgene.18. The process as claimed in claim 12 , wherein the aromatic hydroxyl compound is phenol.19. The process as claimed in claim 12 , wherein the catalyst is pyridine claim 12 , pyridine*HCl claim 12 , TiCl claim 12 , Ti(OPh)or AlCl.20. The process as claimed in claim 12 , wherein the reactor is at least one bubble column reactor.21. The process as claimed in claim 12 , wherein the process is conducted in at least two stages.22. The process as claimed in claim 12 , wherein the phosgene content at the reactor outlet in the liquid phase is less than 100 ppm. The present application relates to a process ...

PROCEDURE FOR THE PREPARATION OF 4-PHENYL BUTYRATE AND USES THEREOF

Provided is a process for preparing 4-phenyl-1-butyric acid, comprising: reacting 4-phenyl-1-butanol with sodium chlorite, a nitroxyl radical catalyst and sodium hypochlorite in an organic solvent and a phosphate buffer; and quenching the reaction with sodium sulfite to produce 4-phenyl-1-butyric. Also provided is 4-phenyl-1-butyric acid prepared by such a process. 1. A compound that is 4-phenyl-1-butyric acid prepared by a process comprising:reacting 4-phenyl-1-butanol with sodium chlorite, a nitroxyl radical catalyst and sodium hypochlorite in an organic solvent and a phosphate buffer; and quenching the reaction with sodium sulfite.2. The compound of claim 1 , wherein said reacting 4-phenyl-1-butanol with sodium chlorite claim 1 , the nitroxyl radical catalyst and sodium hypochlorite in an organic solvent and a phosphate buffer comprises sequentially adding sodium chlorite and sodium hypochlorite to a mixture of 4-phenyl-1-butanol and the nitroxyl radical catalyst in an organic solvent and a phosphate buffer.3. The compound of claim 1 , wherein the nitroxyl radical catalyst is chosen from a TEMPO catalyst and an AZADO catalyst or a mixture thereof.4. The compound of claim 3 , wherein the TEMPO catalyst is chosen from (2 claim 3 ,2 claim 3 ,6 claim 3 ,6-tetramethyl-1-piperidinyloxy claim 3 , free radical) claim 3 , 4-MeO-TEMPO (4-methoxy-2 claim 3 ,2 claim 3 ,6 claim 3 ,6-tetramethylpiperidine-1-oxyl); 4-acetoamido-TEMPO (4-acetamido-2 claim 3 ,2 claim 3 ,6 claim 3 ,6-tetramethylpiperidine-1-oxyl) claim 3 , and 4-hydroxy-TEMPO (4-hydroxy-2 claim 3 ,2 claim 3 ,6 claim 3 ,6-tetramethylpiperidine-1-oxyl).5. The compound of claim 3 , wherein the TEMPO catalyst is polymer-supported.6. The compound of claim 3 , wherein the AZADO catalyst is chosen from 2-azaadamantane N-oxyl (AZADO) claim 3 , 1-methyl-2-azaadamantane-N-oxyl (1-Me-AZADO) claim 3 , and 9-azanoradamantane N-oxyl (Nor-AZADO).7. The compound of claim 3 , wherein the nitroxyl radical catalyst is 9-azabicyclo[3 ...

PROCESS FOR PREPARATION OF HALO SUBSTITUTED BENZOIC ACID COMPOUND AND INTERMEDIATES THEREOF

The present invention provides a process for preparation of halo substituted benzoic acid compound of Formula (1) and intermediates thereof. 4. (canceled)5. The process according to claim 1 , wherein the inorganic base is selected from the group consisting of alkali metal hydroxides claim 1 , alkali earth hydroxides claim 1 , metal carbonates and metal oxides or a mixture thereof.6. The process according to claim 5 , wherein claim 5 , the inorganic base is selected from the group consisting of lithium hydroxide claim 5 , sodium hydroxide claim 5 , potassium hydroxide claim 5 , calcium hydroxide claim 5 , lithium carbonate claim 5 , potassium carbonate claim 5 , sodium carbonate and ammonium carbonate claim 5 , calcium oxide claim 5 , or a mixture thereof.7. The process according to claim 1 , wherein claim 1 , the inorganic sulphate is selected from the group consisting of sodium sulphate claim 1 , potassium sulphate claim 1 , ammonium sulphate claim 1 , calcium sulphate claim 1 , or a mixture thereof.8. The process according to claim 1 , wherein the catalyst is selected from the group consisting of palladium claim 1 , platinum claim 1 , nickel claim 1 , chromium dioxide and Raney nickel supported on alumina or activated carbon.9. The process according to claim 1 , wherein the buffering agent is either a metal phosphate selected from a group consisting of diammonium phosphate claim 1 , mono potassium phosphate claim 1 , dipotassium phosphate claim 1 , magnesium phosphate claim 1 , silver phosphate claim 1 , sodium monofluorophosphate claim 1 , sodium phosphate claim 1 , tripotassium phosphate claim 1 , trisodium phosphate claim 1 , lead(II) phosphate claim 1 , lithium iron phosphate claim 1 , manganese(II) phosphate claim 1 , potassium titanyl phosphate or a metal acetates selected from a group consisting of sodium acetate claim 1 , potassium acetate claim 1 , lithium acetate claim 1 , calcium acetate and magnesium acetate or a mixture thereof. The present invention ...

METHOD FOR PREPARING DIALKYL DICARBONATES USING AMINE OXIDES

The present invention relates to a method for preparing dialkyl dicarbonates from the corresponding alkyl chloroformates using specific amine oxides as catalysts. 2. The method according to claim 1 , wherein Ris selected from the group of straight-chain or branched dodecanyl claim 1 , undecanyl claim 1 , tridecanyl claim 1 , tetradecanyl claim 1 , pentadecanyl claim 1 , hexadecanyl claim 1 , heptadecanyl claim 1 , octadecanyl claim 1 , nonadecanyl claim 1 , eicosanyl claim 1 , icosanyl claim 1 , heneicosanyl and dodoconyl.3. The method according to claim 1 , wherein Ris selected from the group of straight-chain or branched C- claim 1 , C claim 1 , C- claim 1 , C- claim 1 , C- claim 1 , C- claim 1 , C- claim 1 , C- claim 1 , and C-alkyl.4. The method according to claim 1 , wherein Rand Rare selected from the group of methyl claim 1 , ethyl claim 1 , n-propyl claim 1 , s-propyl claim 1 , n-butyl claim 1 , s-butyl claim 1 , isobutyl and t-butyl and Ris straight-chain or branched C-C-alkyl.5. The method according to claim 1 , wherein Rand Rare methyl and Ris C-C-alkyl.6. The method according to claim 1 , wherein Rand Rare methyl and Ris selected from the group of dodecanyl claim 1 , tetradecanyl claim 1 , and hexadecanyl.7. The method according to claim 1 , wherein Ris selected from the group of straight-chain or branched C- claim 1 , C- and C-alkyl and Rand Rare methyl and wherein the content of the compound where R=C-alkyl is from 60% by weight to 80% by weight and the content of the compound where R=C-alkyl is from 19% by weight to 30% by weight and the content of the compound where R=C-alkyl is from 1% by weight to 10% by weight claim 1 , based on the total weight of the compound of the formula (I).9. The method according to claim 8 , wherein Ris methyl claim 8 , ethyl claim 8 , n-propyl claim 8 , isopropyl claim 8 , or n-butyl or isobutyl.10. The method according to claim 1 , wherein the alkali metal hydroxides or alkaline earth metal hydroxides and/or carbonates ...

PROCESS FOR THE PREPARATION OF MONO-PROTECTED ALPHA,OMEGA-DIAMINO ALKANES

The present invention relates to a process for the synthesis of mono-protected α,ω-diamino alkanes, the use of said process in a process for the synthesis of a linker drug comprising an α,ω-diamino alkane moiety and the use of the process of the present invention in a process for preparing an antibody-drug conjugate comprising an α,ω-diamino alkane moiety. 2. The process according to claim 1 , wherein R is Calkyl and Ris selected from H claim 1 , (CH)OCH claim 1 , (CHCHO)H claim 1 , (CHCHO)CH claim 1 , (CH)NHP claim 1 , (CH)N(CH) claim 1 , (CH)NHCONH claim 1 , (CH)NHSOCH claim 1 , (CH)SONH claim 1 , optionally substituted Calkyl claim 1 , optionally substituted Ccycloalkyl and optionally substituted Cheterocycloalkyl.3. The process according to claim 1 , wherein R is CHand Ris selected from (CH)OCH claim 1 , (CHCHO)H claim 1 , (CHCHO)CHand optionally substituted Calkyl.4. The process according to claim 1 , wherein the coupling reagent is selected from the group consisting of carbodiimide reagents claim 1 , phosphonium reagents and aminium reagents.5. The process according to claim 1 , wherein the borane reagent is borane claim 1 , diborane or a borane-ligand complex.6. The process according to claim 5 , wherein the borane reagent is a borane-ligand complex selected from borane tetrahydrofuran or borane dimethyl sulfide.7. The process according to claim 1 , wherein the protective group P is selected from the group consisting of 1 claim 1 ,1-dimethyl-2-haloethyl carbamate claim 1 , 1 claim 1 ,1-dimethyl-2 claim 1 ,2-dibromoethyl carbamate claim 1 , t-butyl carbamate claim 1 , 1-adamantyl carbamate claim 1 , N-(2-pivaloylamino)-1 claim 1 ,1-dimethylethyl carbamate claim 1 , 2-[(2-nitrophenyl)dithio]-1-phenylethyl carbamate claim 1 , 9-anthrylmethyl carbamate claim 1 , methyl carbamate claim 1 , ethyl carbamate claim 1 , p-methoxybenzyl carbamate claim 1 , N-hydroxypiperidinyl claim 1 , p-nitrobenzyl carbamate claim 1 , diphenylmethyl carbamate claim 1 , m-chloro-p- ...

METHOD OF PRODUCING ACID HALIDE SOLUTION AND METHOD OF PRODUCING MONOESTER COMPOUND

Provided is a method of producing an acid halide solution that is useful in production of a polymerizable liquid-crystal compound. The method of producing an acid halide solution includes: a first step of reacting a specific dicarboxylic acid compound with a halogenating agent in a water-immiscible organic solvent in the presence of at least 1.1 equivalents and not more than 3.0 equivalents of an activator relative to the dicarboxylic acid compound to obtain a reaction liquid including a solution that contains an acid halide compound and an oily liquid that is immiscible with the solution containing the acid halide compound; and a second step of removing the oily liquid from the reaction liquid obtained in the first step to obtain a purified liquid containing the acid halide compound. 2. The method of producing an acid halide solution according to claim 1 , further comprisinga third step of, after the second step, concentrating the purified liquid obtained in the second step.5. The method of producing an acid halide solution according to claim 4 , whereinthe nitrogen atom-containing polar aprotic solvent is an amide solvent.6. The method of producing an acid halide solution according to claim 5 , whereinthe amide solvent is at least one selected from the group consisting of N,N-dimethylformamide, N,N-dimethylacetamide, N-methylpyrrolidone, and 1,3-dimethyl-2-imidazolidinone.7. The method of producing an acid halide solution according to claim 4 , whereinthe tetraalkylammonium salt of formula (III) is at least one selected from the group consisting of benzyltriethylammonium chloride, methyltrioctylammonium chloride, tetrabutyl ammonium chloride, and benzyltrimethylammonium chloride.8. The method of producing an acid halide solution according to claim 1 , whereinthe halogenating agent is at least one selected from the group consisting of thionyl chloride, oxalyl chloride, sulfuryl chloride, phosphoryl chloride, phosphorus trichloride, and phosphorus pentachloride.12. ...

NON-PEPTIDE BDNF NEUROTROPHIN MIMETICS

Methods and compounds for treating neurological and other disorders are provided. Included is the administering to a subject in need thereof an effective amount of a compound having binding and/or modulation specificity for a TrkB receptor molecule. 2. The compound of wherein{'sup': 1', '2', '3, 'each of X, X, and Xis —H, —F, or —Cl;'}{'sup': 1', '2', '3, 'sub': 1', '6, 'Ak, Ak, and Akeach independently is optionally substituted C-Calkyl; and'}{'sup': A', 'B', 'A′', 'B′, 'each of R, R, R, and R independently is —H, —F, or —Cl.'}3. The compound of or wherein{'sup': 1', '2', '3, 'each of X, X, and Xis —H;'}{'sup': 1', '2', '3, 'sub': 1', '4, 'Ak, Ak, and Akeach independently is optionally substituted C-Calkyl; and'}{'sup': 1', '2', '3', 'A, 'sub': '2', 'R, R, and Reach independently is —OH, —ORor —NH.'}4. The compound of any one of to wherein{'sup': 1', '2', '3, 'each of X, X, and Xis —H;'}{'sup': 1', '2', '3, 'sub': 2', '3, 'Ak, Ak, and Akeach independently is optionally substituted C-Calkyl; and'}{'sup': 1', '2', '3', 'A', 'A, 'L, L, and Leach independently is —C(O)NH—, —C(S)NH—, —C(O)NR—, or —C(S)NR—; and'}{'sup': 1', '2', '3', 'A, 'sub': '2', 'R, R, and Reach independently is —OH, —ORor —NH.'}5. The compound of any one of to wherein{'sup': 1', '2', '3, 'each of X, X, and Xis —H;'}{'sup': 1', '2', '3, 'sub': 2', '2, 'Ak, Ak, and Akeach is —CH—CH—;'}{'sup': 1', '2', '3', 'A', 'A, 'L, L, and Leach independently is —C(O)NH— or —C(O)NR—, —C(S)NR—; and'}{'sup': 1', '2', '3', 'A, 'sub': '2', 'R, R, and Reach independently is —OH, —ORor —NH.'}6. The compound of any one of to wherein R claim 1 , R claim 1 , and Reach independently is —OR.8. A method of treating a disorder that can be treated by contacting claim 1 , activating or inhibiting a TrkB receptor in a subject in need of treatment thereof claim 1 , comprising administering to the subject an effective amount of a compound of any one of to .9. The method of claim 8 , wherein the disorder is selected from the group ...

PROCESS FOR PREPARATION OF ALKYNYL CARBOXYLIC ACIDS

The invention provides a simple, efficient, environmental friendly catalytic system for the direct carboxylation reaction using COunder mild condition. A single step heterogeneous catalytic process for preparation of alkynyl carboxylic acids of formula I is disclosed. 110-. (canceled)12. The process according to claim 11 , wherein the heterogeneous copper(II) exchanged montmorillonite K-10 catalyst is present in a range of 10-30 w/w %.13. The process according to claim 11 , wherein the base is used in the range of 1-2 equivalents.14. The process according to claim 11 , wherein yield of said alkynyl carboxylic acids of formula I is in the range of 70-94%.15. The process according to claim 11 , wherein selectivity of said alkynyl carboxylic acid is 100%. The present invention relates to a reproducible, environmental friendly single step heterogeneous catalytic process for preparation of alkynyl carboxylic acids. More particularly, the present invention provides a process for preparation of alkynyl carboxylic acids using heterogeneous catalytic system by carboxylation of terminal alkyne by COunder milder reaction conditions in good yield and selectivity.Chemical Fixation of Carbon Dioxide has attracted much attention in view of environmental, legal, and social issues in the past few decades due to increasing levels of carbon dioxide. Carbon dioxide is an attractive C1 building block in organic synthesis because it is an abundant, renewable carbon source and an environmentally friendly chemical reagent. The utilization, as opposed to the storage of COis indeed more attractive especially if the transformation of carbon dioxide to useful bulk products is an economical one. Much research has been devoted toward exploring technologies for COtransformation, whereby harsh and severe reaction conditions are one of the major limitations for their practical applications. Therefore, the development of efficient catalyst systems for COutilization under mild conditions is highly ...

METHOD FOR PREPARING MULTI-SUBSTITUTED ACRYLIC ACID COMPOUND

A method for preparing a multi-substituted acrylic acid compound includes steps as follow. A reaction solution is provided, wherein the reaction solution includes an organometallic reagent, a nickel-containing metal catalyst, a catalyst ligand, a first solvent, and the organometallic reagent is a Grignard reagent or a Gilman reagent. An addition step is conducted, wherein an alkyne compound is mixed with the reaction solution so as to undergo an addition reaction, thus an intermediate solution is obtained. A substitution step is conducted, wherein a carbon dioxide is introduced into the intermediate solution so as to obtain the multi-substituted acrylic acid compound. 2. The method for preparing the multi-substituted acrylic add compound of claim 1 , wherein the nickel-containing catalyst is a nickel halide.3. The method for preparing the multi-substituted acrylic acid compound of claim 1 , wherein the nickel-containing catalyst comprises a nickel halide and a first ligand.4. The method for preparing the multi-substituted acrylic acid compound of claim 3 , wherein the first ligand is dimethoxyethane or bis(2-methoxyethyl) ether.5. The method for preparing the multi-substituted acrylic acid compound of claim 1 , wherein a concentration of the nickel-containing catalyst is 5 mol % to 20 mol % based on 100 mol % of the alkyne compound.6. The method for preparing the multi-substituted acrylic acid compound of claim 1 , wherein the catalyst ligand is a phosphine compound.7. The method for preparing the multi-substituted acrylic acid compound of claim 6 , wherein the catalyst ligand is triphenylphosphine.8. The method for preparing the multi-substituted acrylic acid compound of claim 1 , wherein the first solvent is an aprotic solvent.9. The method for preparing the multi-substituted acrylic add compound of claim 8 , wherein the first solvent is tetrahydrofuran.10. The method for preparing the multi-substituted acrylic acid compound of claim 1 , wherein the addition step ...

PROCESS FOR MAKING LYSINE-GLUTAMIC ACID DIPEPTIDE DERIVATIVES

The invention relates to compounds of the formula 2. The process of claim 1 , wherein the ester protecting group is selected from C-alkyl claim 1 , optionally substituted with phenyl claim 1 , C-alkenyl claim 1 , piperidinyl or dimethylaminoboranyl.3. The process of claim 1 , wherein Ris hydrogen or C-alkyl.4. The process of claim 1 , wherein Ris C-alkyl.5. The process of claim 1 , wherein Ris hydrogen.6. The process of claim 1 , wherein Ris 9H-fluoren-9-ylmethoxycarbonyl7. The process of claim 1 , wherein Ris t-butyl.8. The process of claim 1 , wherein Ris C-alkyl.9. The process of claim 1 , wherein Ris C-alkyl.10. The process of claim 1 , wherein Ris pentadecyl.11. The process of claim 1 , wherein Ris 9H-fluoren-9-ylmethoxycarbonyl and Ris C-alkyl.12. The process of claim 1 , wherein Ris 9H-fluoren-9-ylmethoxycarbonyl and Ris pentadecyl.15. The process of claim 1 , wherein the coupling of the glutamic acid derivative of formula II with the lysine derivative of formula III is carried out by solid phase synthesis.16. The process of claim 1 , wherein the coupling of the glutamic acid derivative of formula II with the lysine derivative of formula III is carried out by FMOC solid phase synthesis. This application is a divisional of U.S. application Ser. No. 14/539,126 filed on Nov. 12, 2014, which is a continuation of PCT/EP2013/059759 filed on May 13, 2013, which claims priority to EP Patent Application No. 12168119.1 filed on May 15, 2012, the disclosures of which are all incorporated herein by reference in their entiretyThe invention relates to compounds of the formulawherein,Rand Rare the same or different and denote hydrogen or an ester protecting group,Ris hydrogen or an amino protecting group andRis C-alkyl,and its enantiomers, diastereomers and salts.The invention in a further embodiment relates to a process for the preparation of the compounds of the formula I and to the use of the compounds of formula I in the solid phase peptide synthesis.The compounds of ...

Synthesis Method for Candesartan Cilexetil Intermediate

A synthesis method for a candesartan cilexetil intermediate represented by formula (II) is provided. The method includes (1) dissolving a compound represented by formula (IV) to an aprotic solvent to obtain a first mixed solution, and dissolving a phase transfer catalyst and an azidation reagent to water to obtain a second mixed solution; (2) dropping the first mixed solution to the second mixed solution for azidation reaction, and after the reaction is ended, standing and layering same to obtain an organic phase containing a compound represented by formula (V); (3) dropping the obtained organic phase containing the compound represented by formula (V) to tertiary butyl alcohol for rearrangement reaction, and after the reaction is ended, concentrating same to obtain a solid or oily material, then adding a crystallizing solvent to the obtained solid or oily material for recrystallization, and separating same to obtain a crystal. 2. The method according to claim 1 , wherein the aprotic solvent is selected from the group consisting of toluene claim 1 , chlorobenzene claim 1 , xylene claim 1 , chloroform claim 1 , 1 claim 1 ,2-dichloroethane and 1 claim 1 ,2-dibromoethane claim 1 , or any combination thereof.3. The method according to claim 1 , wherein the phase transfer catalyst is selected from the group consisting of tetrabutylammonium bromide claim 1 , tetrabutylammonium chloride claim 1 , tetrabutylammonium hydrogen sulfate claim 1 , tetrabutylammonium fluoride and tetrabutylammonium iodide claim 1 , or any combination thereof.4. The method according to claim 1 , wherein a molar ratio of the phase transfer catalyst to the compound represented by formula (IV) is 0.01-0.08:1.5. The method according to claim 1 , wherein the azidation reaction is carried out at −3° C. to 10° C.6. The method according to claim 1 , wherein the rearrangement reaction is carried out at 75° C. to 95° C.7. The method according to claim 1 , wherein a molar ratio of tertiary butyl alcohol to ...

FORMATION OF ALPHA,BETA-UNSATURATED CARBOXYLIC ACIDS AND SALTS THEREOF FROM METALALACTONES AND ANIONIC POLYELECTROLYTES

This disclosure provides for routes of synthesis of acrylic acid and other α,β-unsaturated carboxylic acids and their salts, including catalytic methods. For example, there is provided a process for producing an α,β-unsaturated carboxylic acid or a salt thereof, the process comprising: (1) contacting in any order, a group 8-11 transition metal precursor, an olefin, carbon dioxide, a diluent, and a polyaromatic resin with associated metal cations to provide a reaction mixture; and (2) applying conditions to the reaction mixture suitable to produce the α,β-unsaturated carboxylic acid or a salt thereof. Methods of regenerating the polyaromatic resin with associated metal cations are described. 1. A process for forming an α ,β-unsaturated carboxylic acid or salt thereof , the process comprising (a) a metalalactone comprising a Group 8-10 metal and at least one ligand;', '(b) a diluent; and', '(c) a polyaromatic resin with associated metal cations to provide a reaction mixture; and, '(1) contacting'}(2) applying conditions to the reaction mixture suitable to induce a metalalactone elimination reaction to form the α,β-unsaturated carboxylic acid or a salt thereof.2. The process according to claim 1 , wherein the polyaromatic resin with associated metal cations comprises a metallated phenol-formaldehyde resin claim 1 , a metallated polyhydroxyarene-formaldehyde resin claim 1 , or a metallated polyhydroxyarene- and fluorophenol-formaldehyde resin.3. The process according to claim 1 , wherein the polyaromatic resin with associated metal cations comprises a sodium phenol-formaldehyde resin claim 1 , a potassium phenol-formaldehyde resin claim 1 , a sodium resorcinol- and 2-fluorophenol-formaldehyde resin claim 1 , or a potassium resorcinol- and 2-fluorophenol-formaldehyde resin.4. The process according to claim 1 , wherein the polyaromatic resin with associated metal cations is insoluble in the diluent or the reaction mixture.5. The process according to claim 1 , wherein the ...

PROCESS FOR THE PREPARATION OF AN ANTICONVULSANT COMPOUND

The invention provides a novel method for the preparation of intermediates useful in a process designed to obtain known 1,2,4-triaminobenzene compounds, and in particular a specific compound thereof having known anticonvulsant activity. Unlike known methods, the novel method does not require advance protection of the amino groups present on the substrate. 3) A process according to wherein in a compound of formula (II) claim 1 , (III) or (IIIa) the substituent R is ethyl.4) A process according to claim 1 , wherein the nitrating reaction is carried out by using a nitrating agent claim 1 , typically nitric acid having a concentration from about 30% w/w to about 100% w/w.5) Process according to wherein nitric acid has a concentration of about 65% w/w.6) A process according to wherein the nitrating reaction is carried out in the presence of a solvent.7) A process according to claim 6 , wherein the solvent is a polar aprotic solvent claim 6 , a chlorinated solvent claim 6 , a polar protic solvent claim 6 , typically an aqueous organic or a mineral acid.8) A process according to wherein the mineral acid is acetic acid or concentrated sulfuric acid.9) A process according to wherein the mineral acid is sulfuric acid having a concentration of about 95% w/w.10) A process according to claim 1 , wherein the nitrating reaction is carried out at a temperature ranging from about −10° C. and the solvent reflux temperature claim 1 , preferably between about 0° C. and 25° C.12) A process according to wherein in a compound of formula (II) or a salt thereof R is ethyl and Ris H.15) A process according to wherein in a compound of formula (VI) R is ethyl. The present invention relates to a process for the preparation of intermediates of known 1,2,4-triaminobenzene compounds with anticonvulsant activity, and in particular of a specific compound.The compound ethyl N-[2-amino-4-[(4-fluorophenyl)methylamino] phenyl]carbamate of formula (I), also known as retigabine, is a voltage-dependent ...

METHOD FOR REDUCING HALOGENOBENZOIC ACID ESTER USING RUTHENIUM CARBONYL COMPLEX

An object of the present invention is to provide a method for reducing a halogenobenzoic acid ester, in which dehalogenation is inhibited, by using a readily available catalyst. The method comprises reducing an ester with hydrogen gas by using an aromatic hydrocarbon as a solvent in the presence of a ruthenium complex represented by the following general formula (1): 2. The reduction method according to claim 1 , whereinthe substitution position of the Hal in general formulae (6) and (7) is para to the alkoxycarbonyl group and the hydroxymethyl group.3. The reduction method according to claim 1 , whereinthe aromatic hydrocarbon solvent is selected from toluene, xylene, and mesitylene.4. The reduction method according to claim 2 , whereinthe aromatic hydrocarbon solvent is selected from toluene, xylene, and mesitylene. The present invention relates to a method for reducing a halogenobenzoic acid ester.Dehalogenation is known to occur in production of a halogenobenzyl alcohol by reduction of a halogenobenzoic acid ester with hydrogen gas using a transition metal complex as a catalyst, but there are only a few reports on reduction of halogenobenzoic acid esters. Dalton Trans., 2012, 41, 10136 reports reduction of methyl halogenobenzoates, in which dehalogenation is inhibited, using a ruthenium complex having a PNN pincer-type ligand or the like. However, this reduction has such a problem that since the reaction temperature has to be low, further improvement in the catalyst ratio cannot be expected.An object of the present invention is to provide a method for reducing a halogenobenzoic acid ester, in which dehalogenation is inhibited, by using a ruthenium complex which is readily available as a commercial product or the like.Specifically, the present invention includes the following contents [1] to [3].[1] A reduction method, in which dehalogenation is inhibited, the method comprising reducing a halogenobenzoic acid ester in an aromatic hydrocarbon solvent in the ...

PROCESS FOR PREPARING AN UNSATURATED CARBOXYLIC ACID SALT USING AN ARYLOXIDE

Catalytic process for preparing an α,β-ethylenically unsaturated carboxylic acid salt, wherein an alkene and carbon dioxide are reacted in the presence of a carboxylation catalyst and in the presence of a specific aryloxide to obtain the α,β-ethylenically unsaturated carboxylic acid salt, the carboxylation catalyst being a transition metal complex. The process allows for efficient preparation of α,β-ethylenically unsaturated carboxylic acid derivatives from COand an alkene. 2. The catalytic process according to claim 1 , wherein two vicinal R groups constitute an unsaturated C-hydrocarbylene bridge that is optionally substituted by one to four substituents which are independently selected from the group consisting of F claim 1 , Cl claim 1 , Br claim 1 , I claim 1 , ua C-C-alkyl claim 1 , and a C-C-cycloalkyl.4. The catalytic process according to claim 3 , wherein the aryloxide corresponds to the formula (Ia) claim 3 , in which the sum of p and q is at most 3.5. The catalytic process according to claim 3 , wherein:the aryloxide correspoinds to the formula (Ia);p is at most 1;q is at most 2; andthe sum of p and q is 1 or 2.6. The catalytic process according to claim 3 , wherein Ris a C-C-alkyl or a C-C-cycloalkyl.8. The catalytic process according to claim 7 , wherein:the aryloxide corresponds to formula (Ia-2) or (Ia-3); andx is 1 or 2.9. The catalytic process according to claim 7 , wherein:{'sup': '−', 'the aryloxide corresponds to formula (Ia-2) with F being ortho to O; and'}x is 1 or 2.10. The catalytic process according to claim 1 , wherein the aryloxide is an alkali metal claim 1 , an alkaline earth metal or a zinc aryloxide.11. The catalytic process according to claim 1 , wherein the aryloxide is selected from the group consisting of sodium 2-fluorophenolate claim 1 , sodium 3-fluorophenolate claim 1 , sodium 4-fluorophenolate claim 1 , sodium 2 claim 1 ,6-difluorophenolate claim 1 , sodium 2 claim 1 ,4-difluorophenolate claim 1 , sodium 2-chlorophenolate ...

PROCESS FOR PREPARING AN UNSATURATED CARBOXYLIC ACID SALT

The present invention relates to a catalytic process for preparing an α,β-ethylenically unsaturated carboxylic acid salt, comprising contacting an alkene and carbon dioxide with a carboxylation catalyst being a transition metal complex, an alkoxide, and an organic solvent, to obtain an α,β-ethylenically unsaturated carboxylic acid salt, the organic solvent being incompletely miscible with water at a pressure of 1 bar at at least one temperature T and selected from amides and ureas, T being a temperature in the range from 10° C. to 90° C. 1: A catalytic process , suitable for preparing an α ,β-ethylenically unsaturated carboxylic acid salt , the process comprisingcontacting an alkene and carbon dioxide with a carboxylation catalyst to obtain an α,β-ethylenically unsaturated carboxylic acid salt,wherein the carboxylation catalyst comprises a transition metal complex, an alkoxide, and an organic solvent,wherein the organic solvent is incompletely miscible with water at a pressure of 1 bar at at least one temperature T and is selected from the group consisting of an amide and a urea, T being a temperature in a range from 10° C. to 90° C.2: The catalytic process according to claim 1 , wherein the amide or the urea is linear or cyclic and comprises at least 5 carbon atoms and no nitrogen-bound hydrogen atoms claim 1 ,wherein all of the at least 5 carbon atoms other than the carbonyl carbon atom are saturated.3: The catalytic process according to claim 1 , wherein the organic solvent is an N claim 1 ,N-disubstituted formamide claim 1 , an N claim 1 ,N-disubstituted acetamide claim 1 , an N-substituted 2-pyrrolidone claim 1 , or a 1 claim 1 ,3-disubstituted 2-imidazolidinone.4: The catalytic process according to claim 3 , wherein the organic solvent is selected from the group consisting of N-Methylpyrrolidone claim 3 , N-Ethylpyrrolidone claim 3 , 1 claim 3 ,3-Dimethyl-2-imidazolidinone claim 3 , N-Cyclohexylpyrrolidone claim 3 , N claim 3 ,N-Dibutylformamide claim 3 , N ...

NAPHTHALENEDICARBOXYLIC ACID DICHLORIDE PRODUCTION METHOD

A naphthalenedicarboxylic acid dichloride production method includes causing a reaction between naphthalenedicarboxylic acid and a chlorinating agent at a reaction temperature of 20° C. or higher and 75° C. or lower in presence of a solvent including tetrahydrofuran. The causing a reaction in the naphthalenedicarboxylic acid dichloride production method is preferably performed in presence of N,N-disubstituted formamide. 1. A naphthalenedicarboxylic acid dichloride production method comprising causing a reaction between naphthalenedicarboxylic acid and a chlorinating agent at a reaction temperature of 20° C. or higher and 75° C. or lower in presence of a solvent including tetrahydrofuran.2. The naphthalenedicarboxylic acid dichloride production method according to claim 1 , whereinthe causing a reaction is performed in presence of N,N-disubstituted formamide.3. The naphthalenedicarboxylic acid dichloride production method according to claim 2 , whereinthe N,N-disubstituted formamide is dimethyl formamide or diethyl formamide.4. The naphthalenedicarboxylic acid dichloride production method according to claim 1 , whereinthe chlorinating agent is thionyl chloride or oxalyl chloride.5. The naphthalenedicarboxylic acid dichloride production method according to claim 1 , whereinthe naphthalenedicarboxylic acid is 2,6-naphthalene dicarboxylic acid and naphthalenedicarboxylic acid dichloride is 2,6-naphthalenedicarboxylic acid dichloride, orthe naphthalenedicarboxylic acid is 1,4-naphthalenedicarboxylic acid and naphthalenedicarboxylic acid dichloride is 1,4-naphthalenedicarboxylic acid dichloride. The present application claims priority under 35 U.S.C. § 119 to Japanese Patent Application No. 2018-192612, filed on Oct. 11, 2018. The contents of this application are incorporated herein by reference in their entirety.The present disclosure relates to a naphthalenedicarboxylic acid dichloride production method.Naphthalenedicarboxylic acid dichloride is useful as a resin raw ...

METHOD FOR PREPARING HIGH PURITY MONO-HYDROLYZED ACYL HALIDE COMPOUND

A method for preparing a high purity (e.g. greater than 70 wt. %) mono-hydrolyzed acyl halide compound as a precipitate from solution comprising the steps of preparing a solution comprising: i) at least 80 v/v % of a hydrocarbon solvent, ii) water at a molar concentration greater than its solubility limit within the solvent but less that its solubility limit in solution, iii) a tri-hydrocarbyl phosphate compound, and iv) a polyfunctional acyl halide compound at molar ratio to both water and the tri-hydrocarbyl phosphate compound of at least 1:1. 1. A method for preparing a mono-hydrolyzed acyl halide compound as a precipitate from solution comprising the step of preparing a solution comprising:i) at least 80 v/v % of a hydrocarbon solvent having a water solubility of less than 800 ppm,ii) water at a molar concentration greater than its solubility limit within the solvent but less that its solubility limit in solution,iii) a tri-hydrocarbyl phosphate compound, andiv) a polyfunctional acyl halide compound at molar ratio to both water and the tri-hydrocarbyl phosphate compound of at least 1:1.2. The method of wherein the precipitate comprises at least 70 wt % of the mono-hydrolyzed acyl halide compound.3. The method of wherein the precipitate comprises at least 90 wt % of the mono-hydrolyzed acyl halide compound.4. The method of wherein at least one of the polyfunctional acyl halide compound or water are continuously added to the solution.5. The method of wherein both the polyfunctional acyl halide compound and water are continuously added to the solution.6. The method of wherein the concentration of the polyfunctional acyl halide compound is maintained in the solution at a molar ratio greater than 1:1 with water and at least 2:1 with the tri-hydrocarbyl phosphate compound.7. The method of wherein the concentration of water is maintained in the solution at a concentration greater than its solubility limit within the solvent but less that its solubility limit in ...

SYNTHESIS OF ALPHA,BETA-UNSATURATED CARBOXYLIC ACID (METH)ACRYLATES FROM OLEFINS AND CO2

The invention relates to a method for producing α,β-unsaturated carboxylic acids or salts thereof, comprising a step in which a metallalactone is reacted in a solvent in the presence of a halide; to a composition that comprises α,β-unsaturated carboxylic acids or salts thereof and halide ions; and to the use of said composition for the production of superabsorbent materials or as a monomer composition for producing polymers. 2. The process according to claim 1 , wherein R in formula (I) is H or an alkyl radical having from 1 to 10 carbon atoms.3. The process according to claim 1 , wherein R in formula (I) is H or a methyl radical.4. The process according to claim 1 , wherein E in formula (I) is nickel.5. The process according to claim 1 , wherein L is a bidentate ligand.6. The process according to claim 1 , wherein L is a bisphosphane or bisphosphonate ligand claim 1 , preferably selected from among trialkylbisphosphane claim 1 , dialkylarylbisphosphane claim 1 , alkyldiarylbisphosphane claim 1 , triarylbisphosphane ligands.7. The process according to claim 1 , wherein L is a ligand selected from among bis(di-tert-butylphosphino)ethane claim 1 , bis(dicyclohexylphosphino)ethane or bis(diphenylphosphino)ethane.8. The process according to claim 1 , wherein the halide is an iodide.9. The process according to claim 1 , wherein the halide is selected from among NaI claim 1 , LiI and (nBu)NI.10. The process according to claim 1 , wherein the solvent is selected from among cyclic ethers claim 1 , chlorinated aromatics and aliphatic chlorinated hydrocarbons claim 1 , particularly preferably chloroform claim 1 , chlorobenzene and dichloromethane.11. The process according to claim 1 , wherein the compound of the formula (I) is obtained by reaction of a complex of the formula (II){'br': None, 'sub': 'n', 'EL\u2003\u2003(II)'}with an olefin and carbon dioxide.12. The process according to claim 11 , characterized in that the process is carried out without isolation of the ...

5-BROMO-2-(alpha-HYDROXYPENTYL)BENZOIC ACID SODIUM SALTS IN DIFFERENT CRYSTAL FORMS, AND PREPARATION METHOD THEREOF

The present invention discloses 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt in different crystal forms and the preparation methods thereof, and belongs to the field of pharmaceutical chemistry. Said different crystal forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt include: amorphous 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt, crystal form A of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt, and crystal form B of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt. The different crystal forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt obtained according to the present invention have better stability and water-solubility than the mixed forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt, thus is advantageous for pharmaceutical use. Moreover, the different crystal forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt possess much better therapeutic effect than 5-bromo-2-(α-hydroxypentyl)benzoic acid potassium salt. 1. Crystal form A of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt , defined by a XRPD pattern with the diffraction peaks at 20 values of 5.60 , 16.46 , 16.78 , 18.77 , 21.45 , 32.28 , 33.30 , 33.49 , 34.12 , 36.14 , 36.61 , 37.87 , 40.24 , 41.32 , 43.76 , 44.92 , 45.18 , 47.23 , 55.12 , 56.73 , 57.12 , 62.78 , wherein the error range of 20 value is ±0.2.2. Crystal form B of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt , defined by a XRPD pattern with the diffraction peaks at 20 values of 5.72 , 6.69 , 9.93 , 11.09 , 11.84 , 14.55 , 16.42 , 17.27 , 17.80 , 18.28 , 19.86 , 20.98 , 22.21 , 23.43 , 23.88 , wherein the error range of 2θ value is ±0.2.3. A method for preparing amorphous 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt , the method comprising:placing 6-bromo-3-butyl-1(3H)-isobenzofuranone and sodium hydroxide in a crystallizer to form a mixture,adding tetrahydrofuran and water solvents to the mixture; andreacting the mixture containing the solvents under a water bath at ...

PREPARATION OF HALIDE PRODUCTS

A method for the preparation of an acyl or alkyl halide is described. In particular, the method contains, respectively, reacting a carboxylic acid or an alcohol with a halogenation agent in the presence of a base, wherein the reaction is at least partially carried out in a continuous-flow reactor. 1. Method for the preparation of an acyl halide or alkyl halide , comprising reacting a carboxylic acid or an alcohol , respectively , with a halogenation agent in the presence of a base , wherein the reaction is at least partially carried out in a continuous-flow reactor.2. Method according to claim 1 , wherein the molar ratio of the base to the carboxylic acid or the alcohol ranges between 0.1 and 10 claim 1 , preferably between 0.5 and 5 claim 1 , more preferably between 1 and 3 claim 1 , most preferably about 1.3. Method according to claim 1 , wherein the base comprises an organic base claim 1 , preferably a non-nucleophilic organic base claim 1 , more preferably a non-nucleophilic organic amine claim 1 , most preferably a trialkylamine or pyridine.4. Method according to claim 1 , wherein the base comprises a compound selected from the group consisting of trimethyl amine claim 1 , triethyl amine claim 1 , diisopropylethyl amine claim 1 , N-methyl morpholine claim 1 , N-methyl piperidene claim 1 , 1 claim 1 ,4-dimethylpiperazine pyridine claim 1 , 4-(dimethylamino)pyridine claim 1 , 1 claim 1 ,5-diazabicyclo[4.3.0]non-5-ene claim 1 , 1 claim 1 ,8-diazabicyclo[5.4.0]undec-7-ene claim 1 , 1 claim 1 ,4-diazabicyclo[2.2.2]octane claim 1 , 2 claim 1 ,6-lutidine and their solid supported analogues.5. Method according to claim 1 , wherein the molar ratio of the halogenation agent to the carboxylic acid or the alcohol ranges between 0.1 and 10 claim 1 , preferably between 0.5 and 5 claim 1 , more preferably between 1 and 3 claim 1 , most preferably about 1.6. Method according to claim 1 , wherein the halogenation agent comprises a S—Xor P—Xfunctionality claim 1 , wherein X is a ...

PROCESS FOR THE PRODUCTION OF A FERTILIZER

Process for the production of a compound comprising potassium phosphite comprising the steps of (a) reacting carboxylic acid of the formula R—(C(═O)OH)with phosphorous trichloride (PCl) towards a mixture comprising phosphorous acid (HPO) and acid chloride of the formula R—(C(═O)Cl); wherein R is a linear or branched alkyl or alkanediyl group with 1-20 carbon atoms and n is 1 or 2, (b) subjecting said mixture to a separation step, thereby obtaining (i) a fraction comprising crude phosphorous acid (HPO) and (ii) a fraction comprising acid chloride, (c) combining water, a potassium compound selected from KOH, KHCOand KCO, and the fraction comprising crude phosphorous acid, thereby forming an aqueous solution comprising potassium phosphite, and (d) removing organic compounds from said aqueous solution. 112.-. (canceled)13. A process for producing a compound comprising potassium phosphite of formula KHPOwherein x is an average value in the range 1-2 , the method comprising the steps of:{'sub': n', '3', '3', '3', 'n, 'a. reacting carboxylic acid of the formula R—(C(═O)OH)with phosphorous trichloride (PCl) to make a mixture comprising phosphorous acid (HPO) and acid chloride of the formula R—(C(═O)Cl); wherein R is a linear or branched alkyl or alkanediyl group with 1-20 carbon atoms and n is 1 or 2,'}{'sub': 3', '3, 'b. subjecting said mixture to a separation step, thereby obtaining (i) a fraction comprising crude phosphorous acid (HPO) and (ii) a fraction comprising acid chloride, and'}{'sub': 3', '2', '3, 'c. combining water, a potassium compound selected from KOH, KHCOand KCO, and the fraction comprising crude phosphorous acid, thereby forming an aqueous solution comprising potassium phosphite, and'}d. removing organic compounds from said aqueous solution.14. The process according to claim 13 , wherein in step c) the fraction comprising crude phosphorous acid is dosed to an aqueous solution of the potassium compound.15. The process according to claim 13 , wherein step ...

METHODS FOR CONVERTING FLUORINATED COMPOUNDS

Methods of converting a fluorinated compound into a fluorinated acyl fluoride or derivative thereof, the method including reacting the fluorinated compound with a catalytic amount of at least one transition metal compound and an oxygen-containing compound to form the fluorinated acyl fluoride or derivative thereof. Compounds formed using such methods are also included, including for example and derivatives thereof, or combinations thereof. 1. A method of converting a fluorinated compound into a fluorinated acyl fluoride , the method comprising:reacting the fluorinated compound with a catalytic amount of at least one transition metal compound selected from the group consisting of an oxide, a spinel compound, an oxoperoxo metal compound, and oxoperoxo metal complex with organic complexing agents, and a combination thereof; and an oxygen-containing compound to form the fluorinated acyl fluoride,wherein the transition metal compound comprises Ti, V, Cr, Mn, Fe, Co, Ni, Zr, Nb, Mo, Ru, Rh, Pd, Hf, Ta, W, Re, Os, Ir, Pt, or combinations thereof: and{'sub': 2', '3', '2, 'wherein the wherein the oxygen-containing compound comprises an oxygen-containing gas comprising oxygen (O), ozone O), nitrous oxide (NO), or combinations thereof.'}2. The method according to claim 1 , wherein the fluorinated compound comprises at least one epoxide group.3. The method according to claim 1 , wherein the fluorinated compound comprises at least one ether group.4. The method according to claim 1 , wherein the fluorinated compound is a fluorinated olefin containing compound.56-. (canceled)7. The method according to claim 1 , wherein the fluorinated compound is a partially fluorinated four carbon chain compound claim 1 , partially fluorinated five carbon chain compound claim 1 , partially fluorinated six carbon chain compound claim 1 , perfluorinated four carbon chain compound claim 1 , perfluorinated five carbon chain ...

FORMATION OF ALPHA,BETA-UNSATURATED CARBOXYLIC ACIDS AND SALTS THEREOF FROM METALALACTONES AND ANIONIC POLYELECTROLYTES

This disclosure provides processes for forming acrylic acid and other α,β-unsaturated carboxylic acids and their salts, including catalytic processes, and catalyst systems for effecting the processes. For example, there is provided a catalyst system for producing an α,β-unsaturated carboxylic acid or a salt thereof, the catalyst system comprising: (a) a transition metal precursor compound comprising a Group 8-11 transition metal and at least one first ligand; (b) optionally, at least one second ligand; and (c) an anionic polyaromatic resin with associated metal cations. The catalyst system can further comprise (d) an olefin; (e) carbon dioxide (CO); and (f) a diluent. Methods of regenerating the anionic polyaromatic resin with associated metal cations are described. 1. A catalyst system for producing an α ,β-unsaturated carboxylic acid or a salt thereof , the catalyst system comprising:(a) a transition metal precursor compound comprising a Group 8-11 transition metal and at least one first ligand;(b) optionally, at least one second ligand; and(c) an anionic polyaromatic resin with associated metal cations.2. The catalyst system according to claim 1 , wherein the anionic polyaromatic resin with associated metal cations comprises a metallated phenol-formaldehyde resin claim 1 , a metallated polyhydroxyarene-formaldehyde resin claim 1 , or a metallated polyhydroxyarene- and fluorophenol-formaldehyde resin.3. The catalyst system according to claim 1 , wherein the anionic polyaromatic resin with associated metal cations comprises a sodium phenol-formaldehyde resin claim 1 , a potassium phenol-formaldehyde resin claim 1 , a sodium resorcinol- and 2-fluorophenol-formaldehyde resin claim 1 , or a potassium resorcinol- and 2-fluorophenol-formaldehyde resin.4. The catalyst system according to claim 1 , wherein:a) the first ligand, the second ligand, or both the first ligand and the second ligand is a bidentate ligand; orb) the first ligand, the second ligand, or both the ...

IDENTIFIABLE CHEMICAL PRODUCT

The invention is a process for manufacturing a chemical product which may be later identified and distinguished from similar chemical products, and comprises the steps of (i) forming a reaction mixture comprising chemical intermediate A, chemical intermediate B and marker chemical M (ii) providing the conditions which enable chemical intermediate A and chemical intermediate B to react together to form chemical product C, and for marker chemical M to react either with chemical intermediate A to form a marker product AM or with chemical product C to form a marker product CM (iii) after said reactions have taken place, separating a mixture of product C with product AM and/or a mixture of product C with marker product CM from the reaction mix tune wherein product AM and product CM are both distinguishable from product C by analysis. By using the method of the invention, the marked product is formed in situ and in a mixture with unmarked product. 1. A process for manufacturing a chemical product which may be identified and distinguished from similar chemical products , the process comprising the steps of:forming a reaction mixture comprising chemical intermediate A, chemical intermediate B and marker chemical M;(ii) providing the conditions which enable chemical intermediate A and chemical intermediate B to react together to form chemical product C, and for marker chemical M to react either with chemical intermediate A to form a marker product AM or with chemical product C to form a marker product C; and(iii) after said reactions have taken place, separating a mixture of chemical product C with marker product AM and/or a mixture of chemical product C with marker product CM from the reaction mixture,wherein marker product AM and marker product CM are both distinguishable from chemical product C by analysis of said mixture.2. The process of claim 1 , wherein chemical intermediate B incorporates a functional group capable of reacting with chemical intermediate A and marker ...

5-BROMO-2-(alpha-HYDROXYPENTYL)BENZOIC ACID SODIUM SALTS IN DIFFERENT CRYSTAL FORMS, AND PREPARATION METHOD THEREOF

The present invention discloses 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt in different crystal forms and the preparation methods thereof, and belongs to the field of pharmaceutical chemistry. Said different crystal forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt include: amorphous 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt, crystal form A of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt, and crystal form B of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt. The different crystal forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt obtained according to the present invention have better stability and water-solubility than the mixed forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt, thus is advantageous for pharmaceutical use. Moreover, the different crystal forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt possess much better therapeutic effect than 5-bromo-2-(α-hydroxypentyl)benzoic acid potassium salt. 1. Amorphous 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt , characterized in that it is prepared by the following method: 6-bromo-3-butyl-1(3H)-isobenzofuranone and sodium hydroxide are weighed and placed in a crystallizer , to which tetrahydrofuran and water are added , then the mixture is dissolved and reacted under a water bath at 60° C.; after completion of the reaction , the reaction mixture is distilled under reduced pressure to remove all the solvents to yield amorphous 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt , the XRPD pattern of which has no obvious diffraction peak.2. Crystal form A of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt , characterized in having XRPD pattern with the diffraction peaks at 2θ values of 5.60 , 16.46 , 16.78 , 18.77 , 21.45 , 32.28 , 33.30 , 33.49 , 34.12 , 36.14 , 36.61 , 37.87 , 40.24 , 41.32 , 43.76 , 44.92 , 45.18 , 47.23 , 55.12 , 56.73 , 57.12 , 62.78 , wherein the error range of 2θ value is ±0.2.3. Crystal form B of 5-bromo-2-(α- ...

FORMATION OF ALPHA,BETA-UNSATURATED CARBOXYLIC ACIDS AND SALTS THEREOF FROM METALALACTONES AND ANIONIC POLYELECTROLYTES

This disclosure provides for routes of synthesis of acrylic acid and other α,β-unsaturated carboxylic acids and their salts, including catalytic methods. For example, there is provided a process for producing an α,β-unsaturated carboxylic acid or a salt thereof, the process comprising: (1) contacting in any order, a group 8-11 transition metal precursor, an olefin, carbon dioxide, a diluent, and a polyaromatic resin with associated metal cations to provide a reaction mixture; and (2) applying conditions to the reaction mixture suitable to produce the α,β-unsaturated carboxylic acid or a salt thereof. Methods of regenerating the polyaromatic resin with associated metal cations are described. 1. A process for forming an α ,β-unsaturated carboxylic acid or salt thereof , the process comprising (a) a metalalactone comprising a Group 8-10 metal and at least one ligand;', '(b) a diluent; and', '(c) a polyaromatic resin with associated metal cations to provide a reaction mixture; and, '(1) contacting'}(2) applying conditions to the reaction mixture suitable to induce a metalalactone elimination reaction to form the α,β-unsaturated carboxylic acid or a salt thereof.2. The process according to claim 1 , wherein the polyaromatic resin with associated metal cations comprises a metallated phenol-formaldehyde resin claim 1 , a metallated polyhydroxyarene-formaldehyde resin claim 1 , or a metallated polyhydroxyarene- and fluorophenol-formaldehyde resin.3. The process according to claim 1 , wherein the polyaromatic resin with associated metal cations comprises a sodium phenol-formaldehyde resin claim 1 , a potassium phenol-formaldehyde resin claim 1 , a sodium resorcinol- and 2-fluorophenol-formaldehyde resin claim 1 , or a potassium resorcinol- and 2-fluorophenol-formaldehyde resin.4. The process according to claim 1 , wherein the polyaromatic resin with associated metal cations is insoluble in the diluent or the reaction mixture.5. The process according to claim 1 , wherein the ...

PROCESS FOR THE PRODUCTION OF A FERTILIZER

Process for the production of a compound comprising potassium phosphite comprising the steps of (a) reacting carboxylic acid of the formula R—(C(═O)OH)with phosphorous trichloride (PCl) towards a mixture comprising phosphorous acid (HPO) and acid chloride of the formula R—(C(═O)Cl); wherein R is a linear or branched alkyl or alkanediyl group with 1-20 carbon atoms and n is 1 or 2, (b) subjecting said mixture to a separation step, thereby obtaining (i) a fraction comprising crude phosphorous acid (HPO) and (ii) a fraction comprising acid chloride, (c) combining water, a potassium compound selected from KOH, KHCOand KCO, and the fraction comprising crude phosphorous acid, thereby forming an aqueous solution comprising potassium phosphite, and (d) removing organic compounds from said aqueous solution. 112-. (canceled)1331-. (canceled)32. A process for producing an aqueous solution comprising potassium phosphite chosen from KHPO , KHPO , and combinations thereof , said method comprising the steps of:{'sub': n', '3', '3', '3', 'n, 'a. reacting a carboxylic acid of the formula R—(C(═O)OH)with phosphorous trichloride (PCl) to make a mixture comprising phosphorous acid (HPO) and an acid chloride of the formula R—(C(═O)Cl); wherein R is a linear or branched alkyl or alkanediyl group with 1-20 carbon atoms and n is 1 or 2 or R is a cyclohexyl group and n is 1,'}{'sub': 3', '3, 'b. subjecting the mixture to a separation step, thereby obtaining (i) a fraction comprising crude phosphorous acid (HPO) and (ii) a fraction comprising the acid chloride, and'}{'sub': 3', '2', '3, 'c. combining water, a potassium compound selected from KOH, KHCOand KCO, and the fraction comprising the crude phosphorous acid, thereby forming an aqueous solution comprising the potassium phosphite and having a pH below 5, and'}d. removing organic compounds.33. The process according to claim 32 , wherein in step c) the fraction comprising crude phosphorous acid is dosed to an aqueous solution of the ...

Process for Manufacturing Haloacetamides

The present invention relates to a process for manufacturing haloacetamides of formula (I), 18-. (canceled)10. The process of claim 9 , wherein{'sup': 'A', 'sub': 1', '4', '1', '6', '1', '4, 'Ris H, C-C-alkyl or C-C-alkoxy-C-C-alkyl; and'}{'sup': 'B', 'sub': 1', '4', '1', '6', '1', '4, 'Ris C-C-alkyl or C-C-alkoxy-C-C-alkyl.'}11. The process of claim 9 , wherein sub-step (a) is carried out in the absence of any additional solvent.12. The process claim 9 , wherein in sub-step (a) the halones of formula (II) are initially charged in a reaction vessel and subsequently the oleum is added into the reaction vessel.13. The process of claim 9 , wherein in sub-step (a) the oleum and the halones of formula (II) are reacted in a pressure-vessel.15. The process of claim 9 , wherein sub-step (b) is carried out in an additional solvent selected from ethers claim 9 , or mixtures of ethers with other solvents selected from the group consisting of aliphatic hydrocarbons claim 9 , aromatic hydrocarbons claim 9 , halogenated hydrocarbons claim 9 , nitriles claim 9 , ketones and dipolar aprotic solvents.16. The process of claim 9 , wherein in sub-step (b) the amines of formula (IV) are employed. The invention relates to a process for manufacturing haloacetamides of formula (I), which are valuable intermediates in various chemical manufacturing processes.JP 11080084 teaches a process for the preparation of halogenated acetic acid esters starting from haloalkanes.Rong et al. (J. Org. Chem. 1997, 62, 1576-1577) discloses the synthesis of haloacetamides from the respective haloalkanes via the corresponding bis(dialkylamino)-alkenyles. This process involves several steps and also the use of n-butyllithium.Coe et al. (J. Fluorine Chem. 1985, 27, 71-85) discloses a synthesis of haloacetamides from the epoxides of the pentamer and hexamer oligomers of tetrafluoroethylene via the corresponding halogenated ketone. This process requires pyrolysis conditions and suffers on low yields. Dolbier et ...

GASEOUS F-18 TECHNOLOGIES

Methods, compositions, and systems related to preparing gaseous F-compounds for use in radiolabeling positron emission tomography (PET) tracer precursor compounds are disclosed. [F]fluoride ions produced by conventional methods are converted by reaction with an acid anhydride having the formula: to a gaseous F-compound having the formula: wherein each R is independently a substituted or unsubstituted, straight chain or branched CrC4 alkyl group. The resulting gaseous F-compounds can be produced and stored in close proximity to the production location of the [F]fluoride ions (such as within a cyclotron vault), or easily and efficiently transported long distances with minimal loss of-radioactivity. The gaseous F-compounds, which also can be readily trapped on solid-phase extraction media or in organic solvents such as acetonitrile, provide an alternative source of [F]fluoride for use in the nucleophilic substitution reactions that are used to synthesize a large number of F-labeled PET imaging tracers, including 2-[F]fluoro-2-deoxyglucose (FDG). 3. The method of claim 1 , wherein the gaseous F-compound is anhydrous.4. The method of claim 1 , wherein the step of contacting the composition comprising [F]fluoride ions with the anhydride occurs at a temperature of 50-70° Celsius.5. The method of claim 1 , wherein R is an alkyl group that is substituted with one or more halogen atoms.6. The method of claim 5 , wherein the one or more halogen atoms are selected from the group consisting of fluorine and chlorine.7. The method of claim 6 , wherein R is selected from the group consisting of —CHF claim 6 , —CHCl claim 6 , and —CHFCH.8. The method of claim 1 , wherein R is an unsubstituted alkyl group.9. The method of claim 8 , wherein R is selected from the group consisting of —CH claim 8 , —CHCH claim 8 , —CHCHCH claim 8 , —CH(CH) claim 8 , and —C(CH).10. The method of claim 9 , wherein R is —CH.11. (canceled)12. (canceled)13. (canceled)14. (canceled)15. (canceled)16. (canceled ...

PROCESS FOR PRODUCING CHLOROFORMATE COMPOUND

The present invention provides a method for safely producing a large amount of chloroformate compound with high yield. The chloroformate compound can be produced by mixing and reacting a solution of triphosgene, an amine and an alcohol compound in a flow reactor. The chloroformate compound can also be produced by mixing and reacting a solution of triphosgene with a solution comprising an amine and an alcohol compound in a flow reactor. The amine is preferably tributylamine, and preferably used in an amount of 0.8 to 3 equivalents relative to an amount of the alcohol compound. 1: A process for producing a chloroformate compound , comprising:mixing and reacting a first solution comprising triphosgene with a second solution comprising an amine compound and an alcohol compound in a flow reactor.2: The process according to claim 1 , wherein the amine compound is tributylamine.3: The process according to claim 1 , wherein an amount of the amine compound is 0.8 to 3 equivalents relative to an amount of the alcohol compound.4: The process according to claim 1 , wherein each of the first solution and the second solution comprises a solvent selected from the group consisting of an aromatic hydrocarbon solvent claim 1 , an ether solvent claim 1 , and a combination thereof.5: The process according to claim 1 , wherein each of the first solution and the second solution comprises a solvent selected from the group consisting of toluene claim 1 , tetrahydrofuran claim 1 , and a combination thereof.6: The process according to claim 1 , wherein an amount of the triphosgene is 0.3 to 1 equivalent relative to an amount of the alcohol compound.7: The process according to claim 1 , wherein a flow channel of the flow reactor has a cross-sectional area of 10 mmto 30 cm.8: The process according to claim 1 , wherein a reaction temperature in a flow channel of the flow reactor is 60° C. or lower.9: The process according to claim 1 , wherein a retention time in a flow channel of the flow ...

PROCESS FOR THE PREPARATION OF FLUOROALKYL (ALKYL CARBONATES AND CARBAMATES

Fluoroalkyl alkyl carbonates and fluorosubstituted carbamates which are suitable as additives or solvents in lithium ion batteries are prepared from fluoroalkyl fluoroformates and the respective alcohol or amine. Methanol is the preferred alcohol, dimethylamine and diethylamine are preferred amines. Fluoromethyl methyl carbonate is the preferred compound to be produced. Fluoroalkyl fluoroformates can be prepared from aldehydes and carbonyl fluoride. 1. A fluoroalkyl (fluoro)alkyl carbonate of the general formula (I) , FCHR—OC(O)—OR′ , whereinR is a linear or branched alkyl with 1 to 5 carbon atoms; andR′ is 2,2,2-trifluoroethyl.2. The fluoroalkyl (fluoro)alkyl carbonate according to claim 1 , wherein the fluoroalkyl (fluoro)alkyl carbonate is (1-fluoroethyl)-(2 claim 1 ,2 claim 1 ,2-trifluoroethyl)carbonate or (fluoromethyl)-(2 claim 1 ,2 claim 1 ,2-trifluoroethyl)carbonate.3. The fluoroalkyl (fluoro)alkyl carbonate according to claim 2 , wherein the fluoroalkyl (fluoro)alkyl carbonate is (1-fluoroethyl)-(2 claim 2 ,2 claim 2 ,2-trifluoroethyl)carbonate.4. The fluoroalkyl (fluoro)alkyl carbonate according to claim 2 , wherein the fluoroalkyl (fluoro)alkyl carbonate is (fluoromethyl)-(2 claim 2 ,2 claim 2 ,2-trifluoroethyl)carbonate. This application is a continuation of U.S. application Ser. No. 13/383,543, filed Jan. 30, 2012, which is a U.S. national stage entry under 35 U.S.C. §371 of International Application No. PCT/EP2010/059795, filed Jul. 7, 2008, which claims priority benefit to European Application No. 09165665.2, filed Jul. 16, 2009. The entire contents of these applications are explicitly incorporated herein by this reference.The present invention concerns a process for the preparation of fluoroalkyl (fluoro)alkyl carbonates (i.e. fluoroalkyl alkyl carbonates and fluoroalkyl fluoroalkyl carbonates—the term in brackets denotes an optional fluorine substitution), especially of fluoromethyl methyl carbonate, and fluoroalkyl carbamates.Fluoromethyl methyl ...

PROCESS FOR THE PREPARATION OF A FLUOROLACTION DERIVATIVE

A novel process for the preparation of a fluorolactone derivative of the formula 116.-. (canceled)19. Fluoropropionate derivative of claim 17 , wherein A is A3a.2023.-. (canceled) This application is a continuation of international Application PCT/EP2014/050439, filed Jan. 13, 2014, which claims the benefit of priority to International Application PCT/CN2013/070413, filed Jan. 14, 2013, each of which is incorporated herein by reference in its entirety.The present invention relates to a novel process for the preparation of a fluorolactone derivative of the formulaand of its acylated derivative of formulawherein Rstands for a hydroxy protecting group.The acylated fluorolactones of formula V, particularly the benzoyl derivative with R=benzyl are important precursors for the synthesis of prodrug compounds which have the potential to be potent inhibitors of the Hepatitis C Virus (HCV) NS5B polymerase (PCT Int. Publ. WO 2007/065829).Object of the present invention was to find a selective and sealable synthesis hr the preparation of the fluorolactone of formula I and its acylated derivatives of formula V.The object could be achieved with the synthesis of the present invention as described below.The process of the present invention comprises die preparation of a fluorolactone derivative of the formulacomprising the stepsa) reacting the aldehyde of the formulawith a fluoropropionate derivative of formulawherein A is selected from the chiral moietiesand Ph stands for phenyl to form an aldol adduct of the formulawherein A is as above; andb) subjecting to hydrolysis the aldol adduct of formula IV to give the fluorolactone derivative of the formula I.The term “hydroxy protecting group” used for substituent Rrefers to any substituents conventionally used to hinder the reactivity of the hydroxy group. Suitable hydroxy protecting groups are described in Green T., “Protective Groups in Organic Synthesis”, Chapter 1, John Wiley and Sons, Inc., 1991, 10-142 and can e.g. be selected ...

Method for synthesizing paraphthaloyl chloride through continuous flow in microchannel reactor

The disclosure provides a method for synthesizing paraphthaloyl chloride through terephthalic acid chlorination in a reaction mode of a microchannel continuous flow. Compared with an existing technology, this method has characteristics of accurate control of reaction conditions, high phosgene/triphosgene utilization ratio, low catalyst dosage, high TPA conversion ratio within few tens of seconds of reaction time, high TPC yield and the like. 1. (canceled)2. (canceled)3. (canceled)4. (canceled)5. (canceled)6. (canceled)7. (canceled)8. (canceled)9. (canceled)10. (canceled)11. A method for preparing paraphthaloyl chloride through terephthalic acid chlorination in a microchannel reactor , wherein the method comprises the following steps:(1) a preparation of raw materials:a. firstly melting a paraphthaloyl chloride, and then putting a terephthalic acid and a catalyst into the paraphthaloyl chloride, stirring and mixing to obtain a TPA slurry; andb. melting a solid triphosgene to obtain a triphosgene liquid; or, preparing phosgene;(2) reaction process:in a reaction process, using a continuous flow microchannel reactor, using the TPA slurry as a first flow of a material, and using the triphosgene liquid or the phosgene as a second flow of a material; andrespectively feeding the first flow of the material and the second flow of the material into the microchannel reactor for performing a mixing reaction, to obtain a TPC crude product, absorbing a tail gas by connecting water and alkali.12. The method for preparing the paraphthaloyl chloride through the terephthalic acid chlorination in the microchannel reactor as claimed in claim 11 , wherein the catalyst is one or more in a group formed by N claim 11 ,N-dimethylformamide claim 11 , pyridine and N claim 11 ,N-dimethylacetamide claim 11 , and a dosage of the catalyst is 0.1% -3% of a mass of the TPA.13. The method for preparing the paraphthaloyl chloride through the terephthalic acid chlorination in the microchannel reactor ...

METHOD FOR PRODUCING DIALKYLDICARBONATES USING TERTIARY AMINES AS CATALYSTS

The present invention relates to a method for preparing dialkyl dicarbonates from the corresponding alkyl chloroformates using specific tertiary amines as catalysts. 2. The method as claimed in claim 1 , wherein the at least one tertiary amine of the formula (I) comprises at least one tertiary alkylamine of the formula (I) where:{'sup': '1', 'R=methyl, ethyl, propyl or butyl,'}{'sup': '2', 'sub': 17', '20, 'R=C-C-alkyl, and'}{'sup': '3', 'sub': 2', '3', 'n', '2', '3', '2', '2', '2', 'n', '2', '2', '2, 'R=—[CH—CH(CH)—O]—[CH—CH(CH)]—OH or —[CH—CH—CH—O]—[CH—CH—CH]—OH where n=6 to 10.'}3. The method as claimed in claim 2 , wherein:{'sup': '1', 'R=methyl,'}{'sup': '2', 'sub': '18', 'R=straight-chain C-alkyl, and'}{'sup': '3', 'sub': 2', '2', 'n', '2', '3, 'R=—[CH—CH(CH)—O]—[CH—CH(CH)]—OH where n=8.'}4. The method as claimed in claim 1 , wherein:the catalyst comprises a mixture of two or more different tertiary amines of the formula (I), and{'sup': '3', 'sub': 2', '3', 'n', '2', '3, 'Ris —[CH—(CH(CH))—O]—[CH—(CH(CH))]—OH where n =8, 9, 10 or 11.'}5. The method as claimed in claim 1 , wherein the catalyst comprises a mixture of the tertiary amines of the formula (I) claim 1 , comprising various radicals Rthat are straight-chain or branched C- claim 1 , C- claim 1 , C- claim 1 , C- claim 1 , C- or C-alkyl.7. The method as claimed in claim 1 , wherein the alkali metal hydroxides claim 1 , alkaline earth metal hydroxides and/or carbonates are in the form of aqueous solutions.8. The method as claimed in claim 1 , wherein the at least one water-immiscible organic solvent is selected claim 1 , from the group consisting of aliphatic and aromatic hydrocarbons claim 1 , chlorinated hydrocarbons claim 1 , dialkyl carbonates claim 1 , and water-immiscible ethers and esters.9. The method as claimed in claim 1 , wherein the contacting is done in the presence of 0.001 to 0.5 mol % of the tertiary amines of the formula (I) is claim 1 , based on the alkyl haloformates.10. The method as ...

LIQUID CRYSTAL ALIGNMENT AGENT COMPOSITION, METHOD OF PREPARING LIQUID CRYSTAL ALIGNMENT FILM, AND LIQUID CRYSTAL ALIGNMENT FILM, LIQUID CRYSTAL DISPLAY USING THE SAME

The present invention relates to a liquid crystal alignment agent composition comprising degradable liquid crystal alignment polymer; and a catalyst precursor compound of a specific structure, a method for preparing a liquid crystal alignment film using the same, and a liquid crystal alignment film and a liquid crystal display using the same. 6. The liquid crystal alignment agent composition according to claim 5 , wherein in the Chemical Formula 1-2 claim 5 ,{'sup': a', 'b', 'c', 'i, 'R, R, Rand Rare each independently, a C1-10 alkyl group.'}7. The liquid crystal alignment agent composition according to claim 1 , wherein the catalyst precursor compound represented by the Chemical Formula 1 is included in an amount of 0.1 to 30 parts by weight claim 1 , based on 100 parts by weight of the degradable liquid crystal alignment polymer.8. The liquid crystal alignment agent composition according to claim 1 , wherein a rate of viscosity change of the liquid crystal alignment agent composition according to Mathematical Formula 1 is 5% or less:{'br': None, 'A rate of viscosity change (%)=(viscosity of the liquid crystal alignment agent composition after storage at room temperature for 7 days−initial viscosity of the liquid crystal alignment agent composition)/initial viscosity of the liquid crystal alignment agent composition*100\u2003\u2003[Mathematical Formula 1]'}in the Mathematical Formula 1, the viscosity and the initial viscosity of the liquid crystal alignment agent composition are measured at 25° C., using Ubbelohde Viscometer.10. A method for preparing a liquid crystal alignment film claim 1 ,comprising steps of:{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, 'applying the liquid crystal alignment agent composition of on a substrate to form a coating;'}drying the coating;irradiating light to the coating or rubbing the coating to perform alignment treatment; andheat treating the alignment-treated coating to cure.11. The method according to claim 10 , wherein the ...

5-BROMO-2-(alpha-HYDROXYPENTYL)BENZOIC ACID SODIUM SALTS IN DIFFERENT CRYSTAL FORMS, AND PREPARATION METHOD THEREOF

The present invention discloses 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt in different crystal forms and the preparation methods thereof, and belongs to the field of pharmaceutical chemistry. Said different crystal forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt include: amorphous 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt, crystal form A of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt, and crystal form B of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt. The different crystal forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt obtained according to the present invention have better stability and water-solubility than the mixed forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt, thus is advantageous for pharmaceutical use. Moreover, the different crystal forms of 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt possess much better therapeutic effect than 5-bromo-2-(α-hydroxypentyl)benzoic acid potassium salt. 1. 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt.2. A method of reducing brain tissue injury induced by obstruction of cerebral arteries comprising administering the 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt of .3. A method of reducing brain infarction volume comprising administering the 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt of .4. A method of reducing brain edema volume comprising administering the 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt of .5. A method of preventing and treating heart and brain ischemic diseases comprising administering the 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt of .6. A method of improving heart and brain circulatory disorders comprising administering the 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt of .7. A method of producing antithrombotic effects comprising administering the 5-bromo-2-(α-hydroxypentyl)benzoic acid sodium salt of .8. The method of wherein administration of the 5-bromo-2-(α-hydroxypentyl)benzoic ...

PRODUCTION METHOD FOR 5,5-DI-SUBSTITUTED-4,5-DIHYDROISOXAZOLE

The objective of the present invention is to provide a production method for a 4,5-dihydroisoxazole represented by formula (3), which is safe, industrially desirable, economical, and environmentally friendly. 2. The process according to claim 1 , wherein the reaction of the compound of the formula (1) with hydroxylamine is performed in the presence of water.3. The process according to claim 1 , wherein the reaction of the compound of the formula (1) with hydroxylamine is performed in the presence of 100 mol % or more of water based on 1 mol of the compound of the formula (1).4. The process according to claim 1 , wherein the reaction of the compound of the formula (1) with hydroxylamine is performed in the presence of 100 mol % to 1000 mol % of water based on 1 mol of the compound of the formula (1).5. The process according to claim 1 , wherein the catalyst is an acid catalyst.6. The process according to claim 5 , wherein the acid catalyst is one or more acids selected from the group consisting of mineral acids claim 5 , carboxylic acids claim 5 , and sulfonic acids.7. The process according to claim 5 , wherein the acid catalyst is one or more acids selected from the group consisting of nitric acid claim 5 , trifluoroacetic acid claim 5 , maleic acid claim 5 , and p-toluenesulfonic acid.8. The process according to claim 5 , wherein the acid catalyst is trifluoroacetic acid.9. The process according to claim 1 , wherein the catalyst is an acid-base catalyst.10. The process according to claim 9 , wherein the acid of the acid-base catalyst is one or more acids selected from the group consisting of mineral acids claim 9 , carboxylic acids claim 9 , and sulfonic acids.11. The process according to claim 9 , wherein the acid of the acid-base catalyst is one or more acids selected from the group consisting of nitric acid claim 9 , trifluoroacetic acid claim 9 , maleic acid claim 9 , and p-toluenesulfonic acid.12. The process according to claim 9 , wherein the acid of the acid ...

N,N,N'-Trimethyl-Bis-(Aminoethyl) Ether and its Derivatives as Catalysts for Polyurethanes

The present invention provides compounds produced by the reaction of glycidyl ethers and glycidyl esters with ether compounds including N,N,N′-trimethyl-bis-(aminoethyl) ether. N,N,N′-trimethyl-bis-(aminoethyl) ether and its derivatives can be used as polyurethane catalysts. 132-. (canceled)34. The catalyst composition of claim 33 , further comprising at least one additive selected from at least one cell stabilizer claim 33 , at least one flame retardant claim 33 , at least one chain extender claim 33 , at least one epoxy resin claim 33 , at least one acrylic resin claim 33 , at least one filler claim 33 , at least one pigment claim 33 , or any combination thereof.35. The catalyst composition of claim 33 , wherein the at least one polyol comprises at least one polyether polyol claim 33 , at least one polyester polyol claim 33 , at least one polymer polyol claim 33 , or any combination thereof.36. The catalyst composition of claim 33 , further comprising at least one member selected from the group consisting of triethylenediamine claim 33 , N-methylimidazole claim 33 , 1 claim 33 ,2-dimethylimidazole claim 33 , N-methylmorpholine claim 33 , N-ethylmorpholine claim 33 , trimethylamine N claim 33 ,N′dimethylpiperazine claim 33 , 1 claim 33 ,3 claim 33 ,5-tris(dimethylaminopropyl)hexahydrotriazine claim 33 , 2 claim 33 ,4 claim 33 ,6-tris(dimethylaminomethyl)phenol claim 33 , N-methyldicyclohexylamine claim 33 , pentamethyldipropylene triamine claim 33 , N-methyl-N′-(2-dimethylamino)-ethyl-piperazine claim 33 , tributylamine claim 33 , dimethylaminocyclohexylamine claim 33 , pentamethyldipropylene-triamine claim 33 , triethanolamine claim 33 , dimethylethanolamine claim 33 , tris(3-dimethylamino)propylamine claim 33 , and 1 claim 33 ,8 diazabicyclo[5.4.0] undecene.37. The catalyst composition of claim 33 , further comprising at least one additive selected from at least one cell stabilizer claim 33 , at least one flame retardant claim 33 , at least one epoxy resin claim ...

METATHESIS DEPOLYMERIZATION USING ACRYLATES

Olefin metathesis between an acrylate monomer and a polyene comprising molecule or polymer is employed as a method of cross-metathesizing or depolymerizing the molecule. The metathesis reaction forms a telechelic acrylate molecule that is a monomer, oligomer or polymer. The telechelic acrylate molecule can be employed as a monomer for condensation polymerization. 1. A method of controlled depolymerization comprising:providing a polyene comprising molecule;providing an olefin metathesis catalyst;providing an acrylic monomer;combining the polyene comprising polymer with the olefin metathesis catalyst and the acrylic monomer; andremoving a volatile alkene; wherein an acrylic diene comprising monomer, oligomer, or polymer results, wherein the acrylic diene comprising monomer mixture has a plurality of acrylic units on each of the acrylic diene comprising monomers.2. The method of claim 1 , wherein the polyene comprising molecule is polybutadiene claim 1 , polyisoprene claim 1 , or other polyalkylene diene.3. The method of claim 1 , wherein the polyene comprising molecule is a polyunsaturated naturally occurring oil.4. The method of claim 3 , wherein the polyunsaturated naturally occurring oil is castor oil claim 3 , linseed oil claim 3 , corn oil claim 3 , cotton seed oil claim 3 , peanut oil claim 3 , soybean oil claim 3 , sunflower oil claim 3 , grape seed oil claim 3 , sesame oil claim 3 , or hemp oil.5. The method of claim 1 , wherein the olefin metathesis catalyst comprises Grubb's 1generation catalyst claim 1 , Grubb's 2generation catalyst claim 1 , Hoveyda-Grubb's 1st generation catalyst claim 1 , or Hoveyda-Grubb's 2generation catalyst.6. The method of claim 5 , wherein the olefin metathesis catalyst further comprises CuI.7. The method of claim 1 , wherein the acrylic monomer is an unsubstituted or substituted acrylic acid claim 1 , acryloyl halide claim 1 , acrylate claim 1 , acrylamide claim 1 , or mono acrylic anhydride.8. The method of claim 1 , further ...

PROCATALYST FOR POLYMERIZATION OF OLEFINS

The present invention relates to a procatalyst comprising the compound represented by formula A as an internal electron donor (Formula A), wherein R is hydrogen or a methyl group, N is nitrogen atom; O is oxygen atom; and C is carbon atom. The present invention also relates to a process for preparing said polymerization procatalyst and to a polymerization catalyst system comprising said procatalyst, a co-catalyst and optionally an external electron donor. Furthermore, the present invention relates to a polyolefin obtainable by the process according to the present invention and to the use of the compound of formula A as in internal electron donor in catalysts for polymerization of olefins. 4. The procatalyst according to claim 1 , wherein said procatalyst comprises titanium supported on a solid magnesium-containing support.6. The process according to claim 5 , which process comprises the steps of:{'sup': 4', '4', '1', '4', '1', '4', '1, 'sub': z', '2-z', 'x', '2-x, 'i) contacting a compound RMgXwith an alkoxy- or aryloxy-containing silane compound to give a first intermediate reaction product, being a solid Mg(OR)X, wherein: Rand Rare each a linear, branched or cyclic hydrocarbyl group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups, and one or more combinations thereof; wherein said hydrocarbyl group may be substituted or unsubstituted, and may contain one or more heteroatoms; Xand Xare each independently selected from the group consisting of fluoride (F—), chloride (Cl—), bromide (Br—) or iodide (I—); z is in a range of larger than 0 and smaller than 2, being 0 Подробнее

REDUCTION OF CONTENT OF CARBOXYLIC ACIDS AND DERIVATIVES THEREOF IN OLEUM, DISULFURIC ACID OR CONCENTRATED SULFURIC ACID

The present invention concerns a process for the reduction of content of carboxylic acids and derivatives thereof in oleum, disulfuric acid or concentrated sulfuric acid. The invention further concerns a process for the manufacture of carboxylic acid anhydrides comprising the process for the reduction of content of carboxylic acids and derivatives thereof from oleum, disulfuric acid or concentrated sulfuric acid. 1. A process for the reduction of content of carboxylic acids and derivatives thereof in oleum , disulfuric acid or concentrated sulfuric acid , the process comprising submitting a first fraction comprising oleum , disulfuric acid or concentrated sulfuric acid with a first content of carboxylic acid or at least one derivative thereof to a gas stripping operation in order to obtain a second fraction comprising oleum , disulfuric acid or concentrated sulfuric acid with a second content of carboxylic acid or at least one derivative thereof , wherein the second content of carboxylic acid or at least one derivative thereof in the fraction comprising oleum , disulfuric acid or concentrated sulfuric acid is lower than the first content.2. The process according to claim 1 , wherein carboxylic acid and/or carboxylic acid anhydride is comprised in the first fraction comprising oleum claim 1 , disulfuric acid or concentrated sulfuric acid.3. Process The process according to claim 1 , wherein the carboxylic acid is a halogenated carboxylic acid claim 1 , wherein the halogenated carboxylic acid is a compound of formula (I) HalRC(O)—OH claim 1 , wherein Hal is selected from the group consisting of F claim 1 , Cl and Br claim 1 , and wherein R is independently selected from the group consisting of H claim 1 , F claim 1 , Cl claim 1 , Br claim 1 , alkyl and aryl .4. The process according to claim 3 , wherein Hal is F.5. The process according to claim 4 , wherein the compound of formula (I) is trifluoroacetic acid.6. Process The process according to claim 2 , wherein the ...

METHOD OF CATALYTIC OXIDATION OF LIGNITE USING OXYGEN AS OXIDANT AT ATMOSPHERIC PRESSURE

Disclosed is a method of catalytic oxidation of lignite using oxygen as an oxidant at atmospheric pressure, belonging to a method of mild oxidation of lignite. The method is used to mildly oxidize the lignite using the oxygen as the oxidant under the action of a nitroxide radical catalyst and a metal salt or metal oxide cocatalyst; the process comprises the following steps: pulverizing the lignite to 200 meshes or less, drying a pulverized coal sample at a temperature of 80° C. in vacuum for 10 h, weighing 0.5 g of the treated coal sample, sequentially adding 10 ml of acetic acid, 0.5 mmol of a catalyst and 0.15 to 0.25 mmol of a cocatalyst into a round-bottom flask, connecting a tee joint to an upper orifice of a condenser pipe, replacing oxygen in vacuum for three times so that the round-bottom flask is filled with the oxygen, keeping oxygen pressure at 0.1 MPa, reacting at a temperature of 80° C. to 120° C. for 4 to 12 h; filtering after the reaction is finished; decompressing a filtrate to remove the acetic acid, adding a small amount of ethyl acetate to dissolve, then using an excess CHN/ether solution to esterify for 10 h at room temperature, using 0.45 μm filter paper to filter, and analyzing an esterified product through a gas chromatography-mass spectrometer. The method has the advantages of using the oxygen as the oxidant, having low price, having no toxicity, and achieving environmental protection and mild conditions. 1. A method of a catalytic oxidation of a lignite using oxygen as an oxidant at atmospheric pressure for mildly oxidizing the lignite using the oxygen as the oxidant under an action of a nitroxide radical catalyst and a metal salt or a metal oxide cocatalyst , comprising:pulverizing a lignite to 200 meshes or less;drying the lignite being pulverized at a temperature of 80° C. in vacuum for 10 h;weighing 0.5 g of the lignite being dried;sequentially adding 10 ml of acetic acid, 0.5 mmol of a catalyst, and 0.15˜0.25 mmol of a cocatalyst into a ...

Process

A process for the preparation of a compound of formula (I): which is useful as an intermediate in the preparation of pharmaceutically active compounds.

MALONIC ACID DI-SALTS AND A METHOD FOR PREPARING MALONYL DIHALIDES

A compound of Formula 2 is disclosed 2. A compound of wherein{'sup': 1', '2, 'Ris phenyl optionally substituted with Q and up to 3 substituents independently selected from R;'}{'sup': '2', 'sub': 1', '4', '1', '4', '1', '4', '1', '4, 'each Ris independently halogen, C-Calkyl, C-Chaloalkyl, C-Calkoxy or C-Chaloalkoxy;'}{'sub': 1', '4, 'Q is pyridinyl optionally substituted with up to 2 substituents independently selected from halogen and C-Chaloalkyl; and'}{'sup': A', 'B, 'sub': 4', '2', '3', '3', '2', '2', '2', '3', '3', '2', '2', '2', '2', '2', '2, 'each Mand Mis independently Li, Na, K, NH, NH(CHCH), NH(CHCHCHCH), NH(Bn), NH(cyclohexyl)or NH(phenyl).'}3. A compound of wherein{'sup': 1', '2, 'Ris phenyl optionally substituted with up to 2 substituents independently selected from R;'}{'sup': '2', 'sub': 1', '2', '1', '2', '1', '2', '1', '2, 'each Ris independently halogen, C-Calkyl, C-Chaloalkyl, C-Calkoxy or C-Chaloalkoxy; and'}{'sup': A', 'B, 'sub': 4', '2', '3', '3, 'each Mand Mis independently Na, K, NHor NH(CHCH).'}4. A compound of wherein{'sup': 1', '2, 'Ris phenyl substituted with 2 substituents selected from Rat the 3- and 5-positions;'}{'sup': '2', 'sub': '3', 'each Ris independently Cl or —CF; and'}{'sup': A', 'B, 'sub': '4', 'each Mand Mis independently Na, K or NH.'}5. A compound of wherein{'sup': 1', '2, 'Ris phenyl substituted with 1 substituent selected from Rat the 3-position;'}{'sup': '2', 'sub': 3', '3, 'each Ris independently —CFor —OCF; and'}{'sup': A', 'B, 'sub': '4', 'each Mand Mis independently Na, K or NH.'}7. The method of wherein{'sup': 1', '2, 'Ris phenyl optionally substituted with Q and up to 3 substituents independently selected from R;'}{'sup': '2', 'sub': 1', '4', '1', '4', '1', '4', '1', '4, 'each Ris independently halogen, C-Calkyl, C-Chaloalkyl, C-Calkoxy or C-Chaloalkoxy;'}{'sub': 1', '4, 'Q is pyridinyl optionally substituted with up to 2 substituents independently selected from halogen and C-Chaloalkyl; and'}{'sup': A', 'B, 'sub ...

Synthesis of trifluoroacetyl iodide (tfai) from trifluoroacetyl chloride (tfac) and hydrogen iodide (hi) in a liquid phase reaction

The present disclosure provides a process for making trifluoroacetyl iodide (TFAI) in a liquid phase reaction. Specifically, the present disclosure provides a liquid phase reaction of trifluoroacetyl chloride (TFAC) and hydrogen iodide (HI), with or without a catalyst, to form trifluoroacetyl iodide (TFAI). The reaction may be performed at ambient or elevated temperatures.

PROCESS FOR PREPARATION OF DRONEDARONE BY GRIGNARD REACTION

The invention relates to a novel process for the preparation of dronedarone (I) and pharmaceutically acceptable salts thereof, which comprises reacting of compound of formula (IV) with compound of formula (VI) in a Grignard reaction, and the obtained product is isolated and, if desired, converted into a pharmaceutically acceptable salt thereof. The invention also relates to some novel intermediary compounds and processes for the preparation thereof. 9. The process of claim 1 , wherein step a) further comprises an anhydrous solvent and a catalyst.10. The process of claim 9 , wherein the solvent is THF and the catalyst is FeCl.11. The compound of claim 2 , wherein Rand Rare independently selected from the group consisting of H claim 2 , methyl claim 2 , ethyl claim 2 , methoxy claim 2 , and phenyl.12. The process of claim 3 , wherein the solvent is dichloromethane or n-hexane and wherein step a) further comprises a catalyst.13. The process of claim 3 , wherein the amine is selected from the group consisting of ammonia claim 3 , dimethylamine claim 3 , diethylamine claim 3 , N claim 3 ,O-dimethyl hydroxylamine claim 3 , and aniline.14. The compound of claim 4 , wherein X is Cl.15. The compound of claim 4 , wherein X is Br.16. The compound of claim 6 , wherein X is Cl.17. The compound of claim 6 , wherein X is Br. The invention relates to a novel process for the preparation of dronedarone and pharmaceutically acceptable salts thereof, to novel intermediary compounds used in this process and their preparation.Dronedarone, i.e. N-[2-n-butyl-3-[4-[3-(di-n-butylamino)propoxy]benzoyl]-1-benzofuran-5-yl]-methanesulfonamide, having the formula (I):is a known drug for the treatment of arrhythmia (EPO471609).There are some known processes for the preparation of dronedarone as follows:In EP 0471609 the following scheme is disclosed for the preparation of dronedaroneThe above mentioned patent description discloses some new intermediary compounds, too.In WO 02/48078 the following ...

COMPOUNDS HAVING ANTIBACTERIAL ACTIVITY, PROCESS FOR THEIR PREPARATION AND PHARMACEUTICAL COMPOSITIONS COMPRISING THEM

A pharmaceutically acceptable salt, prodrug or derivative compound of the formula I, wherein Ris selected from H, a (C1-C5) alkyl group and a CORgroup; Ris selected from H, a (C1-C5) alkyl group and a CORgroup; Ris selected from H, a (C1-C5) alkyl group, a (C1-C5)-O-alkyl group, a cycloalkyl of (C5-C6) carbon atoms, an aryl group, and an aryl (C1-C5) alkyl group wherein the aryl group can be an unsubstituted aryl or substituted with one or more Rgroups and an NHCORgroup, or the Rand Rgroups together with N may form a piperidine, morpholine or piperazine group; Ris selected from H and a (C1-C5)alkyl group; Ris selected from an aryl group unsubstituted or substituted with one or more R, linear or branched(C1-C5) alkyl or pyridyne groups and a pyridine group; Ris selected from (C1-C5)alkyl groups, halogen and nitro. 3. A compound according to claim 1 , a pharmaceutically acceptable salt claim 1 , prodrug or derivative thereof claim 1 , having antimicrobial activity.4. A pharmaceutical composition comprising at least one compound according to and pharmaceutically acceptable excipients.5. A pharmaceutical composition comprising at least one compound or pharmaceutically acceptable salt claim 2 , prodrug or derivative thereof claim 2 , according to claim 2 , and pharmaceutically acceptable excipients.6. A pharmaceutical composition comprising at least one compound or pharmaceutically acceptable salt claim 3 , prodrug or derivative thereof claim 3 , according to claim 3 , and pharmaceutically acceptable excipients.7. A pharmaceutical composition comprising at least one compound or pharmaceutically acceptable salt claim 1 , prodrug or derivative thereof claim 1 , according to claim 1 , further comprising at least another therapeutically active substance different from the first compound.8. A method for treating infections claim 1 , comprising the administration of a compound or a pharmaceutically acceptable salt claim 1 , prodrug or derivative thereof claim 1 , according to ...

Distillation process comprising at least two distillation steps to obtain purified halogenated carboxylic acid halide, and use of the purified halogenated carboxylic acid halide

The present invention concerns a process for the obtention of a halogenated carboxylic halide having a reduced content of impurities, a fraction of the halogenated carboxylic halide having a reduced content of impurities, and its use in the manufacture of agriculturally and pharmaceutically active compounds.

OIL-BASED DRILLING FLUIDS CONTAINING AN ALKALINE-EARTH DIAMONDOID COMPOUND AS RHEOLOGY MODIFIER

An oil-based drilling fluid and method of preparing an oil-based drilling fluid are disclosed. The oil-based drilling fluid comprising a base oil continuous phase, an aqueous discontinuous phase, and at least one rheology modifier. The at least one rheology modifier including an alkaline-earth diamondoid compound. The method of preparing the oil-based drilling fluid including mixing a base oil, at least one emulsifier, and at least one wetting agent to form a first mixture, adding and mixing at least one rheology modifier into the first mixture to form a second mixture, adding and mixing at least one fluid-loss control additive into the second mixture to form a third mixture, adding and mixing a brine solution into the third mixture to form a fourth mixture, and adding and mixing a weighting additive into the fourth mixture to form the oil-based drilling fluid.

RECYCLABLE CATALYSTS FOR CHLORINATION OF ORGANIC ACIDS AND ALCOHOLS

The present invention discloses recyclable polymeric catalyst of Formula I, for chlorination of organic acids and alcohols using chlorinating agents such as carbonyl chloride, oxalyl chloride or thionyl chloride, 2. The compounds of Formula I according to claim 1 , wherein the polystyrene backbone is derived from either chloromethyl polystyrene or aminomethyl polystyrene in resin form.3. A process for preparation of the polymer catalyst of Formula I comprising;a) reacting acrylates or iminodiesters with polystyrene backbone to obtain amino diester unit tethered to polystyrene backbone; andb) subjecting the amino diester unit tethered to polystyrene backbone to aminolysis with an amine to obtain the catalyst of formula I.4. The process according to claim 3 , wherein the amine is selected from secondary amine or cyclic secondary amine.5. The process according to claim 3 , wherein the polystyrene backbone is derived from either chloromethyl polystyrene or aminomethyl polystyrene in resin form.6. A process for chlorination of organic acids and alcohols catalyzed by compound of Formula I according to claim 1 , wherein chlorinating reagent is selected from carbonyl chloride claim 1 , thionyl chloride or oxalyl chloride. The invention relates to polymer based catalyst for chlorination. More particularly the invention relates to chlorination of organic acids and alcohols using polymeric catalyst.Acid chlorides are important intermediates for a variety of bulk chemicals ranging from drug molecules to surfactants for personal cleansing.Acid chlorides are synthesized by reacting the organic acids with chlorinating agents such as thionyl chloride (SOCl2), phosgene (COCl2), phosphorus trichloride (PCl3), phosphorus pentachloride (PCl5) or oxalyl chloride (COCl)2. This reaction is preferably carried out in the presence of a catalyst, typically N, N-di-substituted formamides and acetamides. The catalysis by formamide type of catalyst goes via Vilsmeier salt (complex) as depicted ...

PROCESS FOR PREPARING FATTY ACID CHLORIDES AND N-ACYL AMINO ACID SALTS

The invention relates to a process for preparing fatty acid chlorides. In a subsequent step, the fatty acid chlorides can be used to prepare N-acyl amino acid salts. The process comprises the formation of a fatty acid chloride in an amine catalyzed reaction of a fatty acid with phosphorous trichloride, thionyl chloride or phosgene, preferably thionyl chloride. The process for preparing N-acyl amino acid salts further comprises the reaction of the fatty acid chloride with an amino acid or an amino ethane sulfonic acid. 1. A process for preparing a fatty acid chloride of formula R—COCl , wherein R is a linear or branched , saturated alkyl group having from 6 to 30 carbon atoms , or a linear or branched , mono- or polyunsaturated alkenyl group having from 6 to 30 carbon atoms , i. providing a fatty acid of formula R—COOH, and', 'ii. reacting the fatty acid of step i. with phosphorous trichloride, thionyl chloride or phosgene, in the presence of a catalyst to form a fatty acid chloride of formula R—COCl, wherein the catalyst is an amine., 'wherein the process comprises the steps of'}2. The process of claim 1 , wherein the amine is selected from the group consisting of amino acids and amino ethane sulfonic acids.3. The process of claim 1 , wherein the amine is glycine claim 1 , taurine or N-methyl taurine.4. The process of claim 1 , wherein step ii. is carried out with an excess of phosphorous trichloride claim 1 , thionyl chloride or phosgene claim 1 , of at least 5 wt.-% claim 1 , based on the stoichiometric amount of fatty acid.5. The process of claim 1 , wherein step ii. is carried out with an excess of phosphorous trichloride claim 1 , thionyl chloride or phosgene claim 1 , of from 5 to 25% claim 1 , based on the stoichiometric amount of fatty acid.6. The process of claim 1 , wherein step ii. is carried out with an excess of phosphorous trichloride claim 1 , thionyl chloride or phosgene claim 1 , of from 7 to 10% claim 1 , based on the stoichiometric amount of fatty ...

CLEAN PROCESS FOR PREPARING CHLOROFORMYL-SUBSTITUTED BENZENE

Clean process for preparing a chloroformyl-substituted benzene by oxidation of a tail gas hydrogen chloride from a chlorination reaction and a chloroacylation reaction and recycling of the resulting oxidation product chlorine gas into the chlorination reaction. The present invention provides a clean process for preparing a polymer-grade chloroformyl-substituted benzene. 1. A process for preparing a chloroformyl-substituted benzene , comprising (1) reacting a methyl aromatic hydrocarbon of formula (X)CH(CH)or a pendant alkyl chloride thereof with chlorine gas under illumination conditions to prepare a trichloromethyl-substituted benzene and obtain hydrogen chloride as a byproduct , wherein X is a chlorine , bromine , or fluorine atom , a is an integer of 0 , 1 , 2 , 3 , 4 , or 5 , b is an integer of 1 , 2 , 3 , or 4 , and a+b≦6 , and the pendant alkyl chloride is a compound where hydrogen atoms of the pendant alkyl group in the methyl aromatic compound are not completely substituted by chlorine atoms;{'sub': a', '6', '6−a−b', 'b, '(2) reacting the trichloromethyl-substituted benzene with water or a corresponding aromatic acid of formula (X)CH(COOH)to prepare the chloroformyl-substituted benzene and to obtain hydrogen chloride as a byproduct, wherein the corresponding aromatic acid is a substituent on a parent nucleus of the aromatic acid and a substituent on a parent nucleus of the methyl aromatic hydrocarbon or pendant alkyl chloride thereof are located at the same substitution position or corresponding substitution positions, and wherein X is a chlorine, bromine, or fluorine atom, a is an integer selected from 0, 1, 2, 3, 4 and 5, b is an integer selected from 1, 2, 3 and 4, and a+b≦6;'}(3) subjecting a gas stream containing the hydrogen chloride as the byproducts from steps (1) and (2) to catalytic oxidation in one or more reactors to form a product gas stream;(4) separating the product gas steam to obtain a gas stream containing chlorine, a gas stream containing ...

PRODUCTION METHOD OF ASYMMETRIC CHAIN CARBONATE

A method for producing an asymmetric chain carbonate by reacting an alcohol with a halocarbonate ester compound in the presence of a basic magnesium salt. 1. A composition comprising: {'br': None, 'sup': 1', '2, 'ROCOOR\u2003\u2003(3),'}, 'an asymmetric chain carbonate represented by Formula (3){'sup': 1', '2', '1, 'wherein, in Formula (3), Ris an organic group; and Ris an organic group different from R, and'} {'br': None, 'sup': 1', '1, 'ROCOOR\u2003\u2003(4),'}, 'at least one selected from the group consisting of symmetric chain carbonates represented by Formula (4){'sup': '1', 'wherein, in Formula (4), Ris as defined above; and'} {'br': None, 'sup': 2', '2, 'ROCOOR\u2003\u2003(5),'}, 'symmetric chain carbonates represented by Formula (5){'sup': '2', 'wherein, in Formula (5), Ris as defined above.'}2. A composition comprising: {'br': None, 'sup': 1', '2, 'ROCOOR\u2003\u2003(3),'}, 'an asymmetric chain carbonate represented by Formula (3){'sup': 1', '2', '1, 'wherein, in Formula (3), Ris an organic group; and Ris an organic group different from R, and'}water,the composition containing water in an amount of 100 ppm or less. This application is a continuation of U.S. application Ser. No. 15/774,829, filed May 9, 2018, which is a National Stage of International Application No. PCT/JP2016/084621, filed Nov. 22, 2016, which claims priority from Japanese Patent Application No. 2015-229018, filed Nov. 24, 2015, the disclosures of which are incorporated herein by reference in their respective entireties.The present invention relates to a method for producing an asymmetric chain carbonate. The present invention also relates to a composition containing an asymmetric carbonate.Patent Literature 1 reports production of methyl-2,2,2-trifluoroethyl carbonate with a yield of 46% by adding methyl chloroformate to a solution containing 2,2,2-trifluoroethanol, pyridine, and dichloromethane.Patent Literature 2 and Patent Literature 3 describe production of highly purified methyl-2,2, ...

PROCESS FOR PREPARING ISOCYANATES CONTAINING ALKOXYSILANE GROUPS

The invention relates to a process for preparing isocyanate containing alkoxysilane groups, in which, in the sequence of steps A) to D), 2. The process according to claim 1 , wherein in step i) the bottoms material is being wholly or partly discharged from the cleavage apparatus,', 'ii) subjected to thermal treatment and/or purification and/or an aftertreatment in the presence of alcohol and', 'iii) the material removed, after thermal treatment and/or purification and/or aftertreatment in step A), B) or C), is fed in again., 'C) purified alkoxysilano(cyclo)alkylurethane obtained after step B) is thermally cleaved to release isocyanate containing alkoxysilane groups and by-product, leaving bottoms material, while'}3. The process according to claim 1 , wherein the alkoxysilano(cyclo)alkylamine has the formula (1){'br': None, 'sup': 3', '2', '1, 'sub': m', '3-m', '2, 'R(OR)Si—R—NH\u2003\u2003(1)'}{'sup': 3', '2', '1, 'where R, Rand Rare each independently identical or different hydrocarbyl radicals having 1-6 carbon atoms, where these may be linear, branched or cyclic, and m is 0-2.'}4. The process according to claim 1 , wherein the dialkyl carbonate used is selected from the group consisting of dimethyl claim 1 , diethyl claim 1 , dipropyl and dibutyl carbonate.6. The process according to claim 1 , wherein the guanidine base is selected from the group consisting ofa. Barton's base, Murphy's guanidine, 1,5,7-triazabicyclo[4.4.0]dec-5-ene (TBD), pentamethylguanidine, tert-butyltetramethylguanidine (BTMG), and i. of oligocarbodiimides or polycarbodiimides with amines or', 'ii. of polyamines with carbodiimides., 'b. reaction products'}7. The process according to claim 1 , wherein claim 1 , in step i) the catalyst is removed and/or deactivated,', 'ii) low boilers are removed by distillation,', 'iii) solids and/or salt burdens are optionally filtered or centrifuged off, and', 'iv) high boilers are removed via thin-film evaporation., 'B) in the sequence of steps i) to iv),'} ...

DISTILLATION PROCESS COMPRISING AT LEAST TWO DISTILLATION STEPS TO OBTAIN PURIFIED HALOGENATED CARBOXYLIC ACID HALIDE, AND USE OF THE PURIFIED HALOGENATED CARBOXYLIC ACID HALIDE

The present invention concerns a process for the production of a fluorinated carboxylic halide having a reduced content of impurities, a fraction of the fluorinated carboxylic halide having a reduced content of impurities, and its use in the manufacture of agriculturally and pharmaceutically active compounds or their intermediates. 1. A process for the production of a compound of the formula (I) R1-C(O)X having a reduced content of impurities , wherein R1 is CFH , CFor CClF2 and X is a halogen , which process comprises a) subjecting a crude fraction comprising compound of formula (I) R1-C(O)X and impurities to at least two distillation steps , wherein the at least two distillation steps are performed at different temperatures and b) recovering at least a fraction of the compound of the formula (I) having a reduced content of impurities.2. The process according to claim 1 , wherein R1 is CClF2 and X is chlorine.3. The process according to claim 1 , wherein a) comprises at least three distillation steps claim 1 , which consist of a low temperature distillation step claim 1 , a medium temperature distillation step and a high temperature distillation step.4. The process according to claim 3 , wherein the medium temperature distillation step is carried out at a head temperature of at least 5° C. lower than the high temperature distillation step claim 3 , and the low temperature distillation step is carried out at a head temperature of at least 5° C. lower than the medium temperature distillation step.5. The process according to claim 3 , wherein the head temperature difference between the high temperature distillation step and the medium temperature distillation step is from 0.5 to 15° C. claim 3 , and wherein the head temperature difference between the medium temperature distillation step and the low temperature distillation step is from 0.5 to 15° C.6. The process according to claim 3 , wherein the low temperature distillation step is performed first claim 3 , the ...

CRYSTALLINE FORM OF VSN16

The present invention relates to a compound of formula (I) in crystalline form, wherein said compound is in the form of the free base or a pharmaceutically acceptable salt thereof, or a solvate of the free base or salt form thereof. The invention also relates to a pharmaceutical composition containing said crystalline form as an active ingredient, and use thereof in the prevention or treatment of disease. The invention further relates to a process for preparing the crystalline form. 3. A crystalline form according to wherein the compound is the free base.4. The crystalline form of which is characterized by an x-ray powder diffraction pattern having at least two diffraction peaks selected from the following 2[theta] values: 9.53±0.3 claim 2 , 10.35±0.3 claim 2 , 14.21±0.3 claim 2 , 14.35±0.3 claim 2 , 19.02±0.3 claim 2 , 19.18±0.3 claim 2 , 20.11±0.3 claim 2 , 20.34±0.3 claim 2 , 20.63±0.3 claim 2 , 21.55±0.3 claim 2 , 23.91±0.3 claim 2 , 24.03±0.3 claim 2 , 33.89±0.3 claim 2 , 38.48±0.3 claim 2 , 38.71±0.3 claim 2 , 38.89±0.3 claim 2 , 41.83±0.3 and 41.95±0.3.5. The crystalline form of which is characterized by an x-ray powder diffraction pattern having at least two diffraction peaks selected from the following 2[theta] values: 9.53±0.3 claim 2 , 14.21±0.3 claim 2 , 14.35±0.3 claim 2 , 19.02±0.3 claim 2 , 19.18±0.3 claim 2 , 20.34±0.3 claim 2 , 21.55±0.3 claim 2 , 38.71±0.3 and 38.89±0.3.6. The crystalline form of which is characterized by an x-ray powder diffraction pattern having at least two diffraction peaks selected from the following 2[theta] values: 9.53±0.3 claim 2 , 14.21±0.3 claim 2 , 14.35±0.3 claim 2 , 38.71±0.3 and 38.89±0.3.7. The crystalline form of which is characterised by an x-ray powder diffraction pattern having at least three diffraction peaks selected from the 2[theta] values set forth in .8. The crystalline form of which is characterised by an x-ray powder diffraction pattern having at least four diffraction peaks selected from the 2[theta] ...

PROCESS FOR THE MANUFACTURING OF AN ACID HALIDE IN A FLOW REACTOR

The present disclosure relates to a process for the manufacturing of an acid halide, wherein the process comprises the steps of: a) providing a flow reactor comprising a reaction chamber; b) providing reactants comprising: i. a carboxylic acid; ii. a reaction co-agent selected from the group consisting of N,N-disubstituted amides; and iii. a phosphoryl halide; c) incorporating the reactants into the reaction chamber of the flow reactor, wherein the molar ratio of the carboxylic acid to the phosphoryl halide is 1 to at least 0.8, and the molar ratio of the carboxylic acid to the co-agent is 1 to at least 0.5; and d) producing a reaction product stream comprising the acid halide. In another aspect, the present disclosure is directed to the use of a phosphoryl halide for the manufacturing of an acid halide in a flow reactor. 1. A process for the manufacturing of an acid halide , wherein the process comprises the steps of:a) providing a flow reactor comprising a reaction chamber; i. a carboxylic acid;', 'ii. a reaction co-agent selected from the group consisting of N,N-disubstituted amides; and', 'iii. a phosphoryl halide;, 'b) providing reactants comprisingc) incorporating the reactants into the reaction chamber of the flow reactor, wherein the molar ratio of the carboxylic acid to the phosphoryl halide is 1 to at least 0.8, and the molar ratio of the carboxylic acid to the co-agent is 1 to at least 0.5; andd) producing a reaction product stream comprising the acid halide.2. A process according to claim 1 , wherein the temperature of the reaction chamber of the flow reactor is in a range from 10° C. to 80° C. claim 1 , after incorporation of the reactants claim 1 , and in particular the first addition stream claim 1 , the second addition stream claim 1 , and the optional third addition stream into the reaction chamber of the flow reactor.3. A process according to claim 1 , wherein the residence time of the reaction product stream comprising the acid halide in the ...

New process

A process for the preparation of a compound of formula (I): which is useful as an intermediate in the preparation of pharmaceutically active compounds.

Method for producing acid halide solution, mixed solution, and method for producing monoester compound

The present disclosure provides a method for producing an acid halide solution that is useful as a production intermediate or the like that allows industrially advantageous production of a polymerizable liquid crystal compound. The method for producing an acid halide solution of the present disclosure includes a step α of reacting a halogenating agent and a dicarboxylic acid compound in a water-immiscible organic solvent in the presence of a tetraalkylammonium salt to obtain a water-immiscible organic solvent solution including an acid halide, and a step β of concentrating the obtained water-immiscible organic solvent solution.

PRODUCTION METHOD OF ASYMMETRIC CHAIN CARBONATE

A method for producing an asymmetric chain carbonate by reacting an alcohol with a halocarbonate ester compound in the presence of a basic magnesium salt. 2. The production method according to claim 1 ,{'sup': '1', 'wherein Ris an alkyl group having no fluorine atom or an alkyl group having a fluorine atom, and'}{'sup': '2', 'Ris an alkyl group having no fluorine atom or an alkyl group having a fluorine atom.'}4. The production method according to claim 3 ,{'sup': '1', 'wherein Ris an alkyl group having no fluorine atom or an alkyl group having a fluorine atom, and'}{'sup': '2', 'Ris an alkyl group having no fluorine atom or an alkyl group having a fluorine atom.'}5. The production method according to claim 3 ,wherein the inorganic base is at least one selected from the group consisting of carbonates of alkali metals, hydroxides of alkali metals, oxides of magnesium, oxides of alkaline earth metals, hydroxides of magnesium, hydroxides of alkaline earth metals, carbonates of magnesium, carbonates of alkaline earth metals, acetates of magnesium, and acetates of alkaline earth metals.6. The production method according to claim 3 ,wherein the desiccant is at least one selected from the group consisting of neutral calcium salts, zeolite, silica gel, alumina, and activated carbon. The present invention relates to a method for producing an asymmetric chain carbonate. The present invention also relates to a composition containing an asymmetric carbonate.Patent Literature 1 reports production of methyl-2,2,2-trifluoroethyl carbonate with a yield of 46% by adding methyl chloroformate to a solution containing 2,2,2-trifluoroethanol, pyridine, and dichloromethane.Patent Literature 2 and Patent Literature 3 describe production of highly purified methyl-2,2,2-trifluoroethyl carbonate by mixing trifluoroethanol, pyridine, and triglyme, and dropwise adding methyl chlorocarbonate to the mixture to synthesize methyl-2,2,2-trifluoroethyl carbonate, followed by rectification to collect ...

FORMATION OF ALPHA,BETA-UNSATURATED CARBOXYLIC ACIDS AND SALTS THEREOF FROM METALALACTONES AND ANIONIC POLYELECTROLYTES

This disclosure provides routes of synthesis of acrylic acid and other α,β-unsaturated carboxylic acids and their salts, including catalytic methods. In an aspect, there is provided a process for producing an α,β-unsaturated carboxylic acid or a salt thereof, the process comprising: (1) contacting in any order a group 8-11 transition metal precursor compound comprising at least one first ligand, at least one second ligand, an olefin, carbon dioxide, a diluent, and an anionic polyaromatic resin with associated metal cations to provide a reaction mixture; and (2) applying conditions to the reaction mixture suitable to produce the α,β-unsaturated carboxylic acid or a salt thereof. Methods of regenerating the polyaromatic resin with associated metal cations are described. 1. A process for producing an α ,β-unsaturated carboxylic acid or a salt thereof , the process comprising: (i) a group 8-11 transition metal precursor compound comprising at least one first ligand;', '(ii) at least one second ligand;', '(iii) an olefin;', {'sub': '2', '(iv) carbon dioxide (CO);'}, '(v) a diluent; and', '(vi) an anionic polyaromatic resin with associated metal cations to provide a reaction mixture; and, 'a) contacting in any order'}b) applying conditions to the reaction mixture suitable to produce the α,β-unsaturated carboxylic acid or a salt thereof.2. The process according to claim 1 , wherein the anionic polyaromatic resin with associated metal cations comprises a metallated phenol-formaldehyde resin claim 1 , a metallated polyhydroxyarene-formaldehyde resin claim 1 , or a metallated polyhydroxyarene- and fluorophenol-formaldehyde resin.3. The process according to claim 1 , wherein the anionic polyaromatic resin with associated metal cations comprises a sodium phenol-formaldehyde resin claim 1 , a potassium phenol-formaldehyde resin claim 1 , a sodium resorcinol- and 2-fluorophenol-formaldehyde resin claim 1 , or a potassium resorcinol- and 2-fluorophenol-formaldehyde resin.4. The ...

PROCATALYST FOR POLYMERIZATION OF OLEFINS COMPRISING AN AMINOBENZOATE INTERNAL DONOR AND A 1,3-DIETHER INTERNAL DONOR IN A SPECIFIC RATIO

A process for preparing a procatalyst for polymerization of olefins, comprising contacting a magnesium-containing support with a halogen-containing titanium compound, a first internal electron donor represented by Formula A, a second internal electron donor represented by Formula B, and an activator; wherein the molar ratio of the first internal donor to the second internal donor is between 0.01 and 0.7; 2. The process according to claim 1 , wherein the first internal electron donor according to Formula A is selected from the group consisting of 4-[benzoyl(methyl)amino]pentan-2-yl benzoate; 2 claim 1 ,2 claim 1 ,6 claim 1 ,6-tetramethyl-5-(methylamino)heptan-3-ol dibenzoate; 4-[benzoyl (ethyl)amino]pentan-2-yl benzoate and 4-(methylamino)pentan-2-yl bis (4-methoxy)benzoate).3. The process according to claim 1 , wherein the second internal electron donor according to Formula B is selected from the group consisting of 2-isobutyl-2-isobutyl-1 claim 1 ,3-dimethoxypropane claim 1 , 2-ethyl-2-butyl-1 claim 1 ,3-dimethoxypropane claim 1 , 2-isopropyl-2-isopentyl-1 claim 1 ,3-dimethoxypropane and 9 claim 1 ,9-bis-methoxymethyl-fluorene.5. The process according to claim 1 , wherein the first internal electron donor is 4-[benzoyl(methyl)amino]pentan-2-yl benzoate and wherein the second internal electron donor is 9 claim 1 ,9-bis-methoxymethyl-fluorene.6. The process according to claim 1 , wherein the ratio between the first internal electron donor and the second internal electron donor is between 0.05 and 0.65.7. The process according to claim 1 , wherein the first internal electron donor is 4-[benzoyl(methyl)amino]pentan-2-yl benzoate and wherein the second internal electron donor is 9 claim 1 ,9-bis-methoxymethyl-fluorene and the activator is ethylbenzoate and wherein the ratio between the first internal electron donor and the second internal electron donor is between 0.3 and 0.5.8. The process according to claim 1 , wherein the first internal electron donor is 4-[benzoyl( ...

Perfluorinated acid fluorides and preparation thereof

A method for the preparation of a perfluorinated acid fluoride (especially 3-alkoxy propionic acid fluoride) is provided. The method results in high yields of the acid fluoride.

Difluoroalkylaromatics

The present invention relates to 3,4-difluoro-2-alkylaromatics and 2,4-difluoro-3-alkylaromatics, to a process for their preparation and to their use for preparing active ingredients.

他喷他多的中间体的合成与应用

本发明公开了一种他喷他多的关键中间体：（1R,2R）-1-乙基-2-甲基苯乙烷类化合物的制备方法，以及应用这个关键中间体制备他喷他多及衍生物的方法。

Preparation of fluorinated functional compounds

ABSTRACT Fluorinated functional compounds, namely perfluorinated and partially-fluorinated functional compounds, such as perfluorinated and partially-fluorinated carboxylic acids, esters, ketones, alcohols, amides, carboxylic acid fluorides, and derivatives thereof, are prepared by: (a) directly fluorinating a fluorinatable cyclic or acyclic carbonate by contacting the carbonate with fluorine gas in a temperature-controlled reactor to fluorinate the carbonate; and (b) combining the resulting fluorinated carbonate with a reactive nucleophile and allowing the carbonate and the nucleophile to react to form a fluorinated functional derivative of the fluorinated carbonate.

Perfluoroisopropylbenzene derivatives

Perfluoroisopropylbenzene derivatives of the general formula (I) or salts thereof, useful as intermediates or raw materials in the synthesis of various industrial materials including agricultural chemicals, drugs and surfactants, wherein X1 is H, halogeno, formyl, optionally halogenated C1-6 alkyl, C1-6 alkylthio, or the like; X2 is H, halogeno, formyl, hydroxyl, C1-6 alkyl, -C(=O)-R1 (wherein R1 is H, halogeno, hydroxyl, C1-6 alkyl, or NR2R3, with R2 and R3 being each H, C1-6 alkyl, or the like), or the like; X3 is H, halogeno, hydroxyl, cyano, isocyanato, hydrazino, diazo, -C(=O)-R1, -SO2-R4 (wherein R4 is halogeno, hydroxyl, C1-6 alkyl, or NR5R6, with R5 and R6 being each H or C1-6 alkyl), or the like; and X4 is H, halogeno, C1-6 alkyl, or C1-6 alkoxy, with publicly known compounds being excepted.

全氟异丙基苯衍生物

通式(I)的全氟异丙基苯衍生物，适合在合成农用化学品、药物和表面活性剂中作为中间体或原料：其中X 1 为H、卤素、甲酰基、可选地卤代的(C 1 －C 6 )烷基、(C 1 －C 6 )烷硫基等；X 2 为H、卤素、甲酰基、羟基、(C 1 －C 6 )烷基、－C(＝O)－R 1 (其中R 1 为H、卤素、羟基、(C 1 －C 6 )烷基、或NR 2 R 3 (其中R 2 和R 3 均为H、C 1－6 烷基等))等；X 3 为H、卤素、羟基、氰基、异氰酸基、肼基、重氮基、－C(＝O)－R 1 、－SO 2 －R 4 (其中R 4 为卤素、羟基、(C 1 －C 6 )烷基或NR 5 R 6 (其中R 5 和R 6 均为H或(C 1 －C 6 )烷基)等；和X 4 为H、卤素、(C 1 －C 6 )烷基或(C 1 －C 6 )烷氧基，公知的化合物除外。

Perfluoroisopropybenzene derivative

Perfluoroisopropylbenzene derivatives of the general formula (I) or salts thereof, useful as intermediates or raw materials in the synthesis of various industrial materials including agricultural chemicals, drugs and surfactants, wherein X 1 is H, halogeno, formyl, optionally halogenated C 1-6 alkyl, —C(═O)—R 1 (wherein R 1 is H, halogeno, hydroxyl, C 1-6 alkyl, or NR 2 R 3 , with R 2 and R 3 being each H, C 1-6 alkyl, or the like), or the like; X 3 is H, halogeno, hydroxyl, cyano, isocyanato, hydrazino, diazo, —C(═O)—R 1 , —SO 2 —R 4 (wherein R 4 is halogeno, hydroxyl, C 1-6 alkyl, or NR 5 R 6 , with R 5 and R 6 being each H or C 1-6 alkyl), or the like; and X 4 is H, halogeno, C 1-6 alkyl, or C 1-6 alkoxy, with publicly known compounds being excepted.

METHOD OF PURIFYING CARBOXYLIC ACID FLUORIDE

An object is to prevent lowering in the yield of R—COF due to contamination by impurities and thereby to produce a high-purity product of R—COF in a stable manner. According to the present invention, provided are: a method of purifying a carboxylic acid fluoride, comprising a step of removing a hydrogen halide by bringing a carboxylic acid fluoride containing the hydrogen halide into contact with a metal fluoride; a method of producing a high-purity carboxylic acid fluoride, comprising a step of bringing a carboxylic acid fluoride containing a hydrogen halide into contact with a metal fluoride as well as a high-purity carboxylic acid fluoride obtained therefrom; and a method of using a metal fluoride as an adsorbent for a hydrogen halide in a method of removing a hydrogen halide from a carboxylic acid fluoride containing the hydrogen halide. 1. A method of purifying a carboxylic acid fluoride , comprising a step of removing a hydrogen halide by bringing a carboxylic acid fluoride containing the hydrogen halide into contact with a metal fluoride.2. A method of producing a high-purity carboxylic acid fluoride , comprising a step of bringing a carboxylic acid fluoride containing a hydrogen halide into contact with a metal fluoride.3. A method of using a metal fluoride as an adsorbent for a hydrogen halide in a method of removing a hydrogen halide from a carboxylic acid fluoride containing the hydrogen halide.4. The method according to claim 1 , wherein the carboxylic acid fluoride containing a hydrogen halide is a reaction product of a halogen exchange reaction below:{'br': None, 'sup': 1', '1, 'R—COX+HF→R—COF+HX'}{'sup': '1', 'wherein R is a monovalent organic group, a hydrogen atom, or a halogen atom; and Xis a halogen atom excluding fluorine.'}5. The method according to claim 1 , wherein the carboxylic acid fluoride containing a hydrogen halide is a reaction product in a reaction between a carboxylic acid chloride and a metal fluoride.6. The method according to ...

Improved process for the production of ring-fluorinated aromatics

METHODS FOR THE PRODUCTION OF α,β-UNSATURATED CARBOXYLIC ACIDS AND SALTS THEREOF

Processes for producing an α,β-unsaturated carboxylic acid, such as acrylic acid, or a salt thereof, using treated solid oxides are disclosed. The treated solid oxides can be calcined solid oxides, metal-treated solid oxides, or metal-treated chemically-modified solid oxides, illustrative examples of which can include sodium-treated alumina, calcium-treated alumina, zinc-treated alumina, sodium-treated sulfated alumina, sodium-treated fluorided silica-coated alumina, and similar materials.

Methods for the production of , -unsaturated carboxylic acids and salts thereof

Processes for producing an α,β-unsaturated carboxylic acid, such as acrylic acid, or a salt thereof, using treated solid oxides are disclosed. The treated solid oxides can be calcined solid oxides, metal-treated solid oxides, or metal-treated chemically-modified solid oxides, illustrative examples of which can include sodium-treated alumina, calcium-treated alumina, zinc-treated alumina, sodium-treated sulfated alumina, sodium-treated fluorided silica-coated alumina, and similar materials.

Process for the continuous formation of an acid fluoride

Es wird ein Verfahren zur kontinuierlichen Bildung eines Säurefluorids aus CO, HF und einem Olefin beschrieben, bei dem man kontinuierlich alle Reaktanten in einem Bereich hoher Turbulenz vermischt und die vermischten Reaktanten aus dem Bereich hoher Turbulenz in einen kontinuierlichen Reaktor überführt, wo der größte Teil der Reaktion erfolgt. Dies gestattet es, die Reaktanten in billiger Weise zu kombinieren und doch die Bildung einer unzulässig hohen Wärmemenge aus dieser exothermen Reaktion zu verhindern. A process for the continuous formation of an acid fluoride from CO, HF and an olefin is described in which all reactants are continuously mixed in a high turbulence area and the mixed reactants are transferred from the high turbulence area to a continuous reactor where most of the Reaction takes place. This makes it possible to combine the reactants in a cheap way and yet prevent the formation of an unacceptably high amount of heat from this exothermic reaction.

一种白藜芦醇的合成方法

本发明提供了一种白藜芦醇的合成方法，属于天然产物合成技术领域。以3，5‑二甲氧基苯甲酸为原料，经酰氯化反应生成3，5‑二甲氧基苯甲酰氯(12)；12又经酰胺化反应生成3，5‑二甲氧基苯酰胺(13)；13经Hofmann(霍夫曼)降解反应生成3，5‑二甲氧基苯胺(14)；14经桑德迈尔反应生成3,5‑二甲氧基碘苯(15)；15与对甲氧基苯乙烯(23)反应生成3,5,4'‑三甲氧基二苯乙烯(31)，31脱甲基化最终生成白藜芦醇(1)，总收率为23.3％。此方法路线所用试剂廉价易得，后处理简单，使用价格低廉的原料去合成Heck反应所需的两个昂贵的中间体。为白藜芦醇的合成提供了一条新的合成方法。

Patent JPS5440280B2

Processo para fabrico de lohexol

A INVENÇÃO REFERE-SE A UM PROCESSO PARA A PRODUÇÃO DE LOHEXOL POR ALQUILAÇÃO DE 5-ACETAMIDO-N,N'-BIS (2,3-DIHIDROXIPROPILO) -2,4,6-TRIIODOISOFTALAMIDA USANDO O 2-(2-METOXI-ETOXI)-ETANOL COMO SOLVENTE NA PRESENÇA DE UMA BASE, E ISOLANDO OPCIONALMENTE O IOHEXOL BRUTO DA MISTURA DE REACÇÃO. O AGENTE DE ALQUILAÇÃO É PREFERENCIALMENTE O 1-CLORO-2,3-PROPANODIOL E A BASE UM HIDRÓXIDO DE UM METAL ALCALINO, TAL COMO HIDRÓXIDO DE SÓDIO OU HIDRÓXIDO DE POTÁSSIO.

全氟异丙基苯衍生物

通式(I)的全氟异丙基苯衍生物，适合在合成农用化学品、药物和表面活性剂中作为中间体或原料：其中X 1 为H、卤素、甲酰基、可选地卤代的(C 1 -C 6 )烷基、(C 1 -C 6 )烷硫基等；X 2 为H、卤素、甲酰基、羟基、(C 1 -C 6 )烷基、-C(＝O)-R 1 (其中R 1 为H、卤素、羟基、(C 1 -C 6 )烷基、或NR 2 R 3 (其中R 2 和R 3 均为H、C 1-6 烷基等))等；X 3 为H、卤素、羟基、氰基、异氰酸基、肼基、重氮基、-C(＝O)-R 1 、-SO 2 -R 4 (其中R 4 为卤素、羟基、(C 1 -C 6 )烷基或NR 5 R 6 (其中R 5 和R 6 均为H或(C 1 -C 6 )烷基))等；和X 4 为H、卤素、(C 1 -C 6 )烷基或(C 1 -C 6 )烷氧基，公知的化合物除外。

2,5–二甲氧基苯甲酰氯的制备方法

本发明的名称是2,5‑二甲氧基苯甲酰氯的制备方法。所属的技术领域是医药技术。本发明所要解决的技术问题为涉及一种更为先进的2，5‑二甲氧基苯甲酰氯的制备方法。本发明所要解决的技术问题的技术方案的要点是该化合物的一种新的制备方法。

알킬화 방향족 카르복시산 및 아실 할로겐화물의 제조방법

본 발명은 특정 온도 및 입력하에서 상응하는 방향족 탄화소소를 이산화탄소와 반응시키는 것에 의해 수득할 수 있는 하기 일반식(I)의 폴리알킬화 방화족 카르복시산의 제조방법에 관한 것이다. 식 중에서, R 1 , R 2 , R 3 , R 4 , 및 R 5 는 서로 독립해서 수소, C 1 - C 20 알킬, 할로겐 및 C 5 - C 8 시클로알킬이며, 단 치환기 R 1 , R 2 , R 3 , R 4 , R 5 중의 적어도 두개는 알킬 및/또는 시클로알킬이다. 본 발명은 또한 상응하느 아실 할로겐화물을 제조하기 위한 원 포트 반응법에도 관한 것이다.

制备邻－(烷氧羰基)苯甲磺酰氯衍生物的方法

本发明涉及制备邻-(烷氧羰基)苯甲磺酰氯衍生物的方法，更具体地说，本发明涉及制备式1所示的邻-(烷氧羰基)苯甲磺酰氯的新方法，其中用是环状的酯化合物的内酯化合物作为原料，以邻-(氯甲基)苯甲酰氯、邻-(氯甲基)苯甲酸酯衍生物和邻-(烷氧羰基)苯甲基硫代硫酸盐作为中间体，式1化合物是合成磺酰脲类除草剂的重要化合物。在所述通式中，X代表氢、卤素、C 1 -C 6 烷基、C 1 -C 6 卤代烷基、C 1 -C 6 烷氧基、C 1 -C 6 烷氧羰基、硝基或苯基；R代表C 1 -C 6 烷基、C 1 -C 6 卤代烷基或C 3 -C 6 环烷基；n代表1-4的整数，其表示取代基的数目。

Способ получения фторированного сложного эфира, фторированного ацилфторида и фторированного винилового эфира

ÐÎÑÑÈÉÑÊÀß ÔÅÄÅÐÀÖÈß (19) RU (51) ÌÏÊ 7 (11) 2003 125 271 (13) A C 07 C 67/03 ÔÅÄÅÐÀËÜÍÀß ÑËÓÆÁÀ ÏÎ ÈÍÒÅËËÅÊÒÓÀËÜÍÎÉ ÑÎÁÑÒÂÅÍÍÎÑÒÈ, ÏÀÒÅÍÒÀÌ È ÒÎÂÀÐÍÛÌ ÇÍÀÊÀÌ (12) ÇÀßÂÊÀ ÍÀ ÈÇÎÁÐÅÒÅÍÈÅ (21), (22) Çà âêà: 2003125271/04, 16.01.2002 (71) Çà âèòåëü(è): ÀÑÀÕÈ ÃËÀÑÑ ÊÎÌÏÀÍÈ, ËÈÌÈÒÅÄ (JP) (30) Ïðèîðèòåò: 16.01.2001 JP 2001-8252 (43) Äàòà ïóáëèêàöèè çà âêè: 10.01.2005 Áþë. ¹ 1 (86) Çà âêà PCT: JP 02/00236 (16.01.2002) Àäðåñ äë ïåðåïèñêè: 129010, Ìîñêâà, óë. Á.Ñïàññêà , 25, ñòð.3, ÎÎÎ "Þðèäè÷åñêà ôèðìà Ãîðîäèññêèé è Ïàðòíåðû", ïàò.ïîâ. Ã.Á. Åãîðîâîé (74) Ïàòåíòíûé ïîâåðåííûé: Åãîðîâà Ãàëèíà Áîðèñîâíà (54) ÑÏÎÑÎÁ ÏÎËÓ×ÅÍÈß ÔÒÎÐÈÐÎÂÀÍÍÎÃÎ ÑËÎÆÍÎÃÎ ÝÔÈÐÀ, ÔÒÎÐÈÐÎÂÀÍÍÎÃÎ R U Ôîðìóëà èçîáðåòåíè 1. Ñïîñîá ïîëó÷åíè ôòîðèðîâàííîãî ñëîæíîãî ýôèðà (1), êîòîðûé âêëþ÷àåò ñòàäèþ ïåðåýòåðèôèêàöèè, ãäå ôòîðèðîâàííûé ñëîæíûé ýôèð (1) è ñîåäèíåíèå (2) âñòóïàþò â ðåàêöèþ ïåðåýòåðèôèêàöèè ñ îáðàçîâàíèåì ñîåäèíåíè (3), è ñòàäèþ ôòîðèðîâàíè , ãäå ñîåäèíåíèå (3) çàòåì ôòîðèðóþò, ÷òîáû ïîëó÷èòü ôòîðèðîâàííûé ñëîæíûé ýôèð (1) â êîëè÷åñòâå, ïðåâûøàþùåì ìîëüíîå êîëè÷åñòâî äî ïåðåýòåðèôèêàöèè R AF-COOCF2-R AF (1) R A-CH2OH (2) R AF-COOCH2-R A (3) ãäå R A îáîçíà÷àåò îäíîâàëåíòíóþ îðãàíè÷åñêóþ ãðóïïó è R AF îáîçíà÷àåò òàêóþ æå ãðóïïó, êàê R A, èëè îäíîâàëåíòíóþ îðãàíè÷åñêóþ ãðóïïó, ïîëó÷åííóþ ôòîðèðîâàíèåì R A. 2. Ñïîñîá ïîëó÷åíè ôòîðèðîâàííîãî ñëîæíîãî ýôèðà (1) ïî ï.1, ãäå íà ñòàäèè ïåðåýòåðèôèêàöèè, ñàìîå áîëüøåå, äâóêðàòíîå ìîëüíîå êîëè÷åñòâî ñîåäèíåíè (2) âçàèìîäåéñòâóåò ñ ôòîðèðîâàííûì ñëîæíûì ýôèðîì (1). 3. Ñïîñîá ïîëó÷åíè ôòîðèðîâàííîãî ñëîæíîãî ýôèðà (1) ïî ï.1 èëè 2, ãäå íà ñòàäèè ôòîðèðîâàíè ôòîðèðîâàíèå ñîåäèíåíè (3) ïðîâîä ò ââåäåíèåì ãàçîîáðàçíîãî ôòîðà â æèäêóþ ôàçó. 4. Ñïîñîá ïîëó÷åíè ôòîðèðîâàííîãî ñëîæíîãî ýôèðà (1) ïî ï.1 èëè 2, ãäå íà ñòàäèè ôòîðèðîâàíè ôòîðèðîâàíèå ñîåäèíåíè (3) ïðîâîä ò ââåäåíèåì ãàçîîáðàçíîãî ôòîðà â æèäêóþ ôàçó, ñîäåðæàùóþ ðàñòâîðåííûé ôòîðèðîâàííûé ñëîæíûé ýôèð (1) èëè ñëåäóþùèé íèæå ôòîðèðîâàííûé àöèëôòîðèä(4) Ñòðàíèöà: 1 RU A 2 0 0 3 1 2 5 2 7 1 A ...

스클라레올 유도체

본 발명은 하기 일반식( I )의 화합물에 관한 것이다. 상기식에서, R은 10개 이하의 탄소원자를 갖는 분지되거나 분지되지 않은 저급-알킬 및 저급-사이클로알킬 그름으로 구성된 그룹으로부터 선택된다. 본 발명은 또한 풍미를 부여하기 위한 특정한 흡연 조성물, 및 본 발명의 신규한 알킬 스클라레올 디올 카보네이트를 혼입시킴을 포함하는, 예를들면, 흡연 조성물에 풍미를 부여하는 방법에 관한 것이다.

通过氧化气体底物得到的(甲基)丙烯酸的纯化方法

为了对通过催化途径或通过氧化还原途径使气体底物(在制造丙烯酸的情况下，该气体底物由丙烷和/或丙烯和/或丙烯醛组成，而在制造甲基丙烯酸的情况下，该气体底物由异丁烷和/或异丁烯和/或叔丁醇和/或甲基丙烯醛组成)氧化得到的(甲基)丙烯酸进行纯化，将反应气体混合物送入吸收塔(C1)的塔底，而在其塔顶逆流送入至少一种疏水的吸收重溶剂，以在塔(C1)的塔底得到由(甲基)丙烯酸、一种或几种吸收重溶剂、次级反应的重产物和少量醋酸(在制造甲基丙烯酸时是丙烯酸)和水构成的物流(4)；然后将来自塔(C1)的物流(4)送到分离塔(C2)中。操作塔(C1)时重溶剂的流量是送入的气体混合物中(甲基)丙烯酸流量的3～5.6倍，使用在塔顶进料并且没有回流的蒸馏塔作为分离塔(C2)。

含氟酯、含氟酰氟及含氟乙烯醚的制造方法

本发明提供以少的工序数制造含氟酯的方法。该含氟酯的制造方法具有包含通过R AF －COOCF 2 －R AF 和R A －CH 2 OH进行酯交换反应制得R AF －COOCH 2 －R A 的酯交换工序、和通过将其在液相中氟化制得含R AF －COOCF 2 －R AF 的反应生成物的氟化工序的特征。式中，R A 为1价有机基、R AF 为与R A 相同的基、或为R A 被氟化的1价有机基。

Process for producing N-acylamino acid surfactants using N-acylamino acid surfactants or their corresponding anhydrides as catalysts