3,5-ДИАЛКИЛ-4-ОКСИБЕНЗИЛЗАМЕЩЕННЫЕ БЕТА-ДИКАРБОНИЛЬНЫЕ СОЕДИНЕНИЯ, СПОСОБ ИХ ПОЛУЧЕНИЯ (ВАРИАНТЫ), ИХ КОМПЛЕКСНЫЕ ХЕЛАТНЫЕ ПРОИЗВОДНЫЕ

... 1. 3,5 диалкил-4-оксибензилзамещенные β-дикарбонильные соединения общей формулы где R', R" -3,5-диалкил-4-оксибензиловые радикалы, a R1, R2 - насыщенные и/или ненасыщенные алифатические, циклоалифатические, циклоалкилароматические, оксиалкильные, фенольные, амидные, имидные, гетероциклические радикалы, β-дикарбонильное соединение может быть также предельным или непредельным циклическим, бициклическим, гетероциклическим соединением. 2. Способ получения 3,5-диалкил-4-оксибензил-замещенных β-дикарбонильных соединений, включающий взаимодействие β-дикарбонильного соединения с алкилирующим агентом в присутствии органического растворителя в щелочной среде, отличающийся тем, что в качестве алкилирующего агента используют N, N-замещенный-3,5-диалкил-4-оксибензилдитиокарбамидат. 3. Способ получения 3,5-диалкил-4-оксибензилзамещенных β-дикарбонильных соединений, включающий взаимодействие β -дикарбонильного соединения с алкилирующим агентом в присутствии органического растворителя в щелочной среде, ...

Способ получения моно- или бис-(дифторметокси)-производных ароматических альдегидов

... 1. СПОСОБ ПОЛУЧЕНИЯ МОНОИЛИ БИС-(ДИФТОРМЕТОКСИ)-ПРОИЗВОДНЫХ АРОМАТИЧЕСКИХ АЛЬДЕГИДОВ общей форО мулы н (OdHTe), -п где п - 0,1m - 1,2, отличающийся тем, что, с целью упрощения технологии процесса, повышения выхода целевого продукта и расширения ассортимента исходных и целевых продуктов, соответствующие моно- или диоксиальдегиды обрабатывают дифторхлорметаном в водно-диоксаО ) новой среде при 60-70С в присутствии едкого натра, взятого в количестве CZ 6-10 моль на 1 моль исходного альдегид;а . 2. Способ ПОП.1, отличающийся тем, что гфоцесс осуществляют в присутствии дигидрата гидросернистокислого натрия при молярном соотношении оксиальдегид:дигидрат гидросернистокислого натрия, равном сю 1: ...

Alpha-Methylencyclopentanon-Derivate und Verfahren zu ihrer Herstellung

PROCESS FOR THE PREPARATION OF CYCLOHEXENE DERIVATIVES, AND A STARTING PRODUCT AND INTERMEDIARY PRODUCTS IN THIS PROCESS

Hydroxycarbonylderivate und Verfahren zu ihrer Herstellung.

TRIPHENYLPHOSPHIN-DERIVATE, DIESE ENTHALTENDE PALLADIUM- ODER NICKEL-KOMPLEXE UND VERFAHREN ZUR HERSTELLUNG VON BIARYL-DERIVATEN

HETEROCYCLISCHE VERBINDUNGEN.

Indane compounds with smooth muscle relaxing and/or mast cell stabilising and/or anti-inflammatory activity

Polysubstituted derivatives of naphthalene a process for preparing them and their use in the pharmaceutical and cosmetic fields

New 2,6-disubstituted derivatives of naphthalene have the formula (I) wherein n is 1 or 2, R1 to R4 are hydrogen or CH3, R5 is (ii)CN, (iv) 2-oxazolinyl, wherein m is 0 or 1, R6 is hydrogen, alkyl, OR9 wherein R9 is H, alkyl or wherein R10 is alkyl or aryl, or R6 is when m=1, r' and r'' representing H, alkyl, mono- or poly-hydroxyalkyl, aryl or a heterocycle when taken together, R7 is H or alkyl, R8 is H, alkyl and the acetal of said compounds, and the salts of the compounds of formula I. These compounds are usefully employed in the pharmaceutical and cosmetic fields.

PROCESS FOR THE SYNTHESIS OF 3-KETO-CYCLOPENTENE-5-OXY DERIVATIVES HAVING INSECTICIDE ACTIVITY

OXIRANE COMPOUNDS

BENZYLPYRIMIDINES

5,6,7-Trimethoxy naphthalene-(2)-carboxylic acid and hydronaphthalene-(2)-carboxylic acid derivatives

Compounds corresponding to the general formula in which the hydrogenated 6-ring may also contain one or two double bonds and in which R<1> is a hydroxy group, a C1-C6alkoxy group, a halogen atom, a C2-C6-alkanoyloxy group, an amino group, a C1-C6-alkylamino group or a dialkylamino group with alkyl radicals of 1 to 6 carbon atoms, the alkyl radicals of the dialkylamino group also being capable of forming with the nitrogen atom a saturated heterocyclic 5- to 7-membered ring which may also contain an oxygen atom or another nitrogen atom, and the salts of these compounds show lipid-reducing properties and in particular produce a distinct reduction in the cholesterol level of hypercholesterolaemic mice. Some of the compounds show psychopharmacological activity and some are vasodilators.

Process for ther solid phase synthesis of aldehyde ketone oxim amine hydroxamic acid abd a b-unsaturated carboxyxlix acid and aldehyde compounds

Process for the solid phase synthesis of of aldehyde, ketone, oxine, amine, hydroxamic acid and B-unsaturated carboxylic acid and aldehyde compounds.

This invention is directed to a process for the solid phase synthesis of aldehyde, ketone, oxime, amine, hydroxamic acid and a,b-unsaturated carboxylic acid and aldehyde compounds and to polymeric hydroxylamine resin compounds useful therefor.

Process for the solid phase synthesis of aldehydes ketones oximes amines and hydroxamic acid compounds

Process for the solid phase synthesis of aldehydes, ketones, oximes, amines and hydroxamic acid compounds.

Process for the solid phase synthesis of aldehyde,ketone, oxime, amine, hydroxamic acid and alpha, b eta-unsaturated carboxylic acid and aldehyde compounds.

Process for the solid phase synthesis of aldehydesketones oximes amines and hydroxamic acid compoun ds

Process for ther solid phase synthesis of aldehyde ketone oxim amine hydroxamic acid abd a b-unsaturated carboxyxlix acid and aldehyde compounds

Process for the solid phase synthesis of aldehydes ketones oximes amines and hydroxamic acid compounds

VERFAHREN ZUR HERSTELLUNG VON NEUEN PHENAN- THRENEN

PROCEDURE FOR THE PRODUCTION OF NEW PHENAN THRENEN

PROCEDURE FOR THE PRODUCTION OF IRONE.

PROCEDURE FOR SUBSTITUTING AROMATIC ORGANIC DERIVATIVES.

AZOLYLMETHYL TETRAHYDROFURANES OF DERIVATIVES, AS PLANT WAX MODULATORS AND FUNGICIDES.

PROCEDURE FOR the PRODUCTION OF 4HYDROXYBENZOPHENONEN.

DRUG, DERIVED FROM 3-HYDROXYDODECAHYDRO-BENZ (E) INDEN-7-ON, PRODUCTS, DERIVED FROM 3-HYDROXY-DODECAHYDRO-BENZ (E) INDEN-7-ON AND PROCEDURE FOR YOUR PRODUCTION.

PROCEDURE FOR the PRODUCTION OF (6-METHOXY-2NAPHTHYL) - (1-BROM|THYL) - KETON AND ITS DERIVATIVES.

NEW AMINODERIVATE the 5 (2-HYDROXYSTYRYL) ISOXAZOLS, PROCEDURES FOR YOUR PRODUCTION AND THESE CONTAINING THERAPEUTIC MEANS.

Procedure for the production optically active Diketobicycloalkane

PROCEDURE FOR THE PRODUCTION OF INTERMEDIATE PRODUCTS

Substituted hydroxyacetophenon derivatives

PYRIDINONE DERIVATIVES

D-AMINO ACID AMIDES

Perfluororalkylation of carbonyl compounds

The present invention provides a process for producing a compound comprising a perfluorinated alkyl group moiety from a carbonyl compound. Typically, the process includes contacting a carbonyl compound with a silane compound in the presence of a fluorohydrogenate ionic liquid under conditions sufficient to produce a compound comprising a perfluorinated alkyl group. The silane compound includes a perfluoroalkyl group.

Purification of carboxaldehyde

Process for the preparation of 2-hydroxyalkyl halophenones

PROCESS FOR THE PREPARATION OF 2-HYDROXYALKYL HALOPHENONES

A process is provided for the preparation of compounds of Formula (1); wherein X1 and X2 are each independently H, Cl or F, provided that at least one of X1 and X2 is Cl or F; one of R1 and R2 is H and the other is OH; and R5 is an unsubstituted alkyl, preferably a C1-6 alkyl, group. The process comprises condensing a 2-chloroalkanoic acid with an optionally substituted benzyl alcohol to form a 2-(optionally substituted benzyloxy) alkanoic acid, converting the condensation product to the corresponding acid chloride and then either reacting the acid chloride with a compound of Formula (2) in the presence of a source of copper (I) to give a compound of Formula (3) wherein one of R3 and R4 is H and the other is optionally substituted benzyloxy; or reacting the acid chloride with a compound of the Formula (4): A-NH-B wherein A and B independently represent substituted alkyl, alkoxy, aryl or oxyaryl groups, or are linked to form a heterocyclic ring to form an amide, and then reacting the amide ...

HYPOTENSIVE AGENT OUDENONE ITS SALTS AND PROCESSES FOR PRODUCTION AND PREPARATION THEREOF

OLIGOMERIC BENZIL KETALS AND THEIR USE AS PHOTOINITIATORS

Compounds of the formula I (see fig. I) in which n is 1-30 and X, Y, R, Ar1 and Ar2 are as defined in claim 1 can be prepared by reaction of a benzil dialkyl ketal with a diol. Depending on the molar ratio of the two reaction components, products having a different polycondensation degree n are obtained. The compounds can be used as photoinitiators.

AMINO DERIVATIVES OF 5-(2-HYDROXYSTYRYL)-ISOXAZOLE, THEIR PREPARATION AND THERAPEUTIC FORMULATIONS CONTAINING THESE COMPOUNDS

The prevent invention is directed to novel aminopropanol derivatives of 5-(2-hydroxystyryl)-isoxazole of the formula (I) (I) where n is 1 or 2, o is 1, 2 or 3, R1 and R2 are each hydrogen or straight-chain or branched alkyl of 1 to 5 carbon atoms, R3 is hydrogen, hydroxyl, halogen alkyl, alkoxy or alkylthio of 1 to 5 carbon atoms, (the last-mentioned three groups each being unsubstituted, or mono-, di or tri-substituted by halogen or mono-substituted by hydroxyl or alkoxy of 1 to 3 carbon atoms), alkenyl, alkynyl, alkynyloxy or cycloalkoxy, each of 2 to 6 carbon atoms in the alkyl and of 3 to 8 carbon atoms in the ring or amino which is unsubstituted or is monoor di-substituted by alkyl of 1 to 5 carbon atoms, and if o is 2 or 3, the R3's may be identical or different, or R3 is methylenedioxy or alkylene of 3 or 4 carbon ? o , and R4 is alkyl of 1 to 4 carbon atoms, and their addition salts with acids. This invention is also concerned with the preparation of said novel compounds, ...

2,6-DISUBSTITUTED NAPHTHALENE DERIVATIVES AND PROCESS FOR PREPARING THE SAME

PROCESS FOR SUBSTITUTION OF AROMATIC ORGANIC COMPOUNDS

METAL-CATALYZED ASYMMETRIC 1,4-CONJUGATE ADDITION OF VINYLBORON COMPOUNDS TO 2-SUBSTITUTED-4-OXY- CYCLOPENT-2-EN-1-ONES YIELDING PROSTAGLANDINS AND PROSTAGLANDIN ANALOGS

This invention provides a novel method for the preparation of 2,3- disubstituted-4-oxy-cyclopentan-l-one compounds that are useful for the synthesis of prostaglandins and prostaglandin analogs of industrial relevance. The method comprises the metal -catalyzed asymmetric 1,4-conjugate addition of vinylboron compounds to 2- substituted-4-oxy-cyclopent-2-en-l-ones. This method relies on the use of less toxic, easily- handled reagents, and can be performed under milder conditions than offered by some conventional methods, affording 2,3-disubstituted-4-oxy-cyclopentan-l-one compounds enantio- and diastereoselectively, which are precursors to the said prostaglandin and prostaglandin analogs, in high yield.

4-CHLORO-4-ALKOXY-1,1,1-TRIFLUORO-2-BUTANONES, THEIR PREPARATION AND THEIR USE IN PREPARING 4-ALKOXY-1,1,1-TRIFLUORO-3-BUTEN-2-ONES

... 4-Chloro-4-alkoxy-1,1,1-trifluoro-2-butanones, prepared by reacting alkyl vinyl ethers with trifluoroacetyl chloride, are useful for preparing 4-alkoxy- 1,1,1-trifluoro-3- buten-2-ones.

ANTIFUNGAL AGENTS, PROCESSES FOR THE PREPARATION THEREOF, AND INTERMEDIATES

A compound represented by the general formula: (see formula 1) wherein R1 and R2 denote a halogen atom or hydrogen atom; R3 means a hydrogen atom or lower alkyl group; ~ , r and m stand for 0 or 1; A is N or CH; W denotes an aromatic ring or a condensed ring thereof; X means another aromatic ring, an alkanediyl group, an alkenediyl group, or an alkynediyl group; Y stand for -S-, etc.; Z denotes a hydrogen atom, etc., or a salt thereof, and intermediates thereof or a salt thereof as well as processes for the preparation thereof, and pharmacetical composition suitable for use as an antifungal agent.

INDANE DIMER COMPOUNDS AND THEIR PHARMACEUTICAL USE

Indame dimer compounds and their pharmaceutical use particularly to achieve smooth muscle relaxing activity and/or mast cell stabilising activity and/or anti-inflammatory activity are described. ...

Verfahren zur Herstellung fester Formaldehydlösungen.

Phenanthrene compounds anti-androgens

Phenanthrene compounds of general formula (I), of which the left hand side corresponds to parts 2-4 and the right hand side to parts 5-7, and their salts and quaternary compounds. R1=H-, C1-4 alkyl, alkenyl- or alkynyl- R2=H-, methyl- R3=H-, C1-4 alkyl-, alkenyl- or alkynyl- X=presence or absence of -CH2- R4=H-, acyl- or O, N-group next to ketone e.g oxime ketal or R5 = C1-4 alkyl-, alkenyl-, alkynyl- Z=tert.amino-, acyloxy-, C1-4 alkyloxy- dotted line = presence or absence of a double bond (R1)=absence of R1 if there is a double bond at 4a for instance compound Anti-androgen, anti-myogen, anti-thymolytic without other hormone activity. For treatment of hirsutism.

VERFAHREN ZUR HERSTELLUNG VON OUDENON.

VERFAHREN ZUR HERSTELLUNG VON OPTISCH AKTIVEN BICYCLISCHEN DIKETONEN.

Dicarbonyl compds and 21-alkanoyl-pregna- - 4-ene-3, 20-diones prepn

Dicarbonyl compds and 21-alkanoyl-pregna-4-ene-3,20-diones prepn. Compds (I): (where R' is R1CO or CM; R" is R2CO R3OCO or CM; R1R2 and R4-R8 are H or organic residues; R3 is an organic residue; one or more of R1R2 and R4-R8 may be linked to form a cyclic residue >4C and n, and R2 are 0, 1 or 2) are prepd. simply and in good yield by treating a compd. (II) with a stony base and opt. a thiophilic agent esp. a trivalent P-compd. Prefd., products are steroids and esp. compd (III) (which are anti-inflammatory agents) and their 1,2-satd. nor derivs and DELTA, 135 (10)-triene steroids carrying a (III) 3-free, etherified or esterified OH and where R1 is an opt substd hydrocarbon; R2 is H, OH or OAcyl; R3 is H, OH, OAcyl or Me; R2 + R3 may be a bond or alkylene- or cycloalkylene-dioxy; R4 is H, Cl, OH or OAcyl; R4 + R5 may be O; R6 is Ha Hal; R4 + R6 may be a hond or epoxy; R7 is H, Me or Ha and R8 is H or when 1,2 is present H or Cl.

Dicarbonyl compds and 21-alkanoyl-pregna- - 4-ene-3, 20-diones prepn

Dicarbonyl compds and 21-alkanoyl-pregna-4-ene-3,20-diones prepn. Compds (I): (where R' is R1CO or CM; R" is R2CO R3OCO or CM; R1R2 and R4-R8 are H or organic residues; R3 is an organic residue; one or more of R1R2 and R4-R8 may be linked to form a cyclic residue >4C and n, and R2 are 0, 1 or 2) are prepd. simply and in good yield by treating a compd. (II) with a stony base and opt. a thiophilic agent esp. a trivalent P-compd. Prefd., products are steroids and esp. compd (III) (which are anti-inflammatory agents) and their 1,2-satd. nor derivs and DELTA, 135 (10)-triene steroids carrying a (III) 3-free, etherified or esterified OH and where R1 is an opt substd hydrocarbon; R2 is H, OH or OAcyl; R3 is H, OH, OAcyl or Me; R2 + R3 may be a bond or alkylene- or cycloalkylene-dioxy; R4 is H, Cl, OH or OAcyl; R4 + R5 may be O; R6 is Ha Hal; R4 + R6 may be a hond or epoxy; R7 is H, Me or Ha and R8 is H or when 1,2 is present H or Cl.

[...] D' iNVERSION DE L' [...].

1.9-TO-[...] AND MEDICAMENT CONTAINING THEM.

CYCLOHEXADIEN DERIVATIVES AND PROCEDURES FOR THE PRODUCTION THE SAME.

NOVEL METHOD FOR THE SYNTHESIS OF THE 3 KETO 5 HYDROXY-CYCLOPENTEN.

Disubstituted ethanes

Compounds of the formula in which R<2> is one of the groups -R<3>, -OR<3>, -CO-R<3>, -CO-OR<3> and -O-CO-R<3>, R<1> and R<3> are straight-chain alkyl groups having 1 to 12 carbon atoms, and n is one of the numbers 1 and 2, their preparation, mixtures which contain such compounds, and the use in electro-optical devices are described. The novel compounds of the formula I are particularly useful as components in liquid-crystal mixtures and for the most part themselves have liquid-crystalline properties.

Process for the preparation of anthrone

Anthrone is prepared by an intramolecular condensation of a hydroanthraquinone, e.g. tetrahydroanthraquinone or dihydroanthraquinone, by heating in the absence of oxygen.

Benzylpyrimidines and process for their preparation

Novel 2,4-diamino-5-benzylpyrimidines of the formula in which R<1> and R<2> represent a C1-6-alkyl radical, R<3> represents a C1-3-alkyl radical and R<4> represents methylene or a C2-4-alkylidene radical, and their physiologically tolerable acid addition salts, potentiate the antibacterial action of sulphonamides. The compounds of the formula I can be prepared in various ways.

POLY-SUBSTITUTED NAPHTHALENE DERIVATIVES, PROCESS FOR THEIR PREPARATION AND PHARMACEUTICAL AND COSMETIC COMPOSITIONS CONTAINING THEM.

PROCEDURE FOR the PRODUCTION OF 2-CYCLOPENTENONEN.

2.6-DISUBSTITUTED NAPHTHALENE DERIVATIVES, PROCESS FOR THEIR PREPARATION AND PHARMACEUTICAL OR COSMETIC CONTAINING THEM.

PURIFICATION OF CARBOXALDEHYDE DERIVATIVES

СПОСОБ ТВЕРДОФАЗНОГО СИНТЕЗА АЛЬДЕГИДА, КЕТОНА, ОКСИМА, АМИНА, ГИДРОКСАМОВОЙ КИСЛОТЫ И α, β-НЕНАСЫЩЕННОЙ КИСЛОТЫ И АЛЬДЕГИДНЫХ СОЕДИНЕНИЙ

Данное изобретение относится к способу твердофазного синтеза альдегида, кетона, оксима, амина, гидроксамовой кислоты и α,β-ненасыщенной карбоновой кислоты и альдегидных соединений и к используемым для этого полимерным соединениям гидроксиламиносмол. Отчет о международном поиске был опубликован 2000.04.06 ...

ФУНГИЦИДНЫЕ 2-МЕТОКСИБЕНЗОФЕНОНЫ

... 1. Соединение формулы I где R1обозначает атом галогена или С1-С10алкильную группу; R2обозначает атом водорода, галогена, С1-С10алкил, C1-С10алкокси- или нитрогруппу, или R1и R2вместе обозначают группу формулы -СН=СН-СН=СН-; R3и R4, каждый независимо, обозначают С1-С10алкильную или бензильную группу, необязательно замещенную одним или несколькими атомами галогена, нитро- или цианогруппой, циклоС1-С10алкилом, галогенС1-С10алкилом, галогенциклоС1-С10алкилом, С1-С10алкокси, галогенС1-С10 алкокси, фенилом, галоген- или дигалогенфенилом или пиридилом; и n равно целому числу от 0 до 3. 2. Соединение по п.1, где R1обозначает атом хлора или метильную группу; R2обозначает атом водорода, хлора или брома; R3обозначает С1-5алкильную группу; R4обозначает С1-5 алкильную группу или группу бензила, необязательно замещенную, по меньшей мере, атомом галогена или С1-4алкилом или алкоксигруппой; и n равно 0. 3. Соединение по п.2, выбранное из группы, состоящей из 6,6'-диметил-2,2',3',4'-тетраметоксибензофенона ...

СПОСОБ ПОЛУЧЕНИЯ 2,2-ДИ/2-ПРОПОКСИ/-1-ФЕНИЛЕТАНОНА

Данное изобретение относится к способам получения 2,2-ди-(2-пропокси)-1-фенилетанона, который применяется как фотоинициатор для фотополи-меризационноспособных композиций, которые применяются в радиоэлектронной, лакокрасочной, полиграфической и других отраслях промышленности. Способ получения 2,2-ди-(2-пропокси)-1-фенилетанона в две стадии, на первой из которых в водный раствор ацетофенона, который содержит кислоту, при температуре 50-70 °С в течение 3-8 часов порциями вводят окислитель - нитрит натрия 1 выдерживают реакционную массу при 70-80 °С в течение 1-3 часов с получением фенилглиоксаля и его взаимодействием на второй стадии с избытком пропанола-2 в азеотропообразующем растворителе при температуре кипения азеотропной смеси до прекращения выделения воды.

A PROCESS FOR THE SOLID PHASE SYNTHESIS OF ALDEHYDE OF a, b- UNSATURATED ALKENOATE RESIN

ШТАМ HALOBACTERIUM HALOBIUM 353П - ПРОДУЦЕНТ БІЛКОВО-ВІТАМІННОЇ БІОМАСИ

Штам Halobacterium halobium 353П - продуцент білково-вітамінної біомаси.

METHOD OF SOLID-PHASE SYNTHESIS OF ALDEHYDES, KETONES, OXIMES, AMINES AND HYDRO KSAMOVOI ACID

Simple method for dehalogenating alpha-halogenated compounds

Method for synthesizing diaryl ether by using amino acid as additive

PROCESS FOR PREPARATION OF 2,3-DIFLUOROBENZENES

METHOD FOR CREATING CARBON-CARBON BONDS, NON-CATALYSIS, FROM CARBONYL COMPOUNDS

La présente invention concerne un procédé de préparation d'un composé de formule (I) par réaction entre un composé de formule (II) et un composé de formule (III) en l'absence de catalyseur notamment de catalyseur métallique, et de ligand, et en présence d'une base L'invention concerne également l'utilisation de ce procédé pour la préparation de composés d'intérêt, notamment du Tamoxifen.

SULPHONATES Of OPTICALLY ACTIVE ALLETHROLONE, THEIR METHOD OF PREPARATION AND THEIR APPLICATION TO the INVERSION OF the CENTER Of ASYMMETRY Of the ALLETHROLONE

PROCESS OF SYNTHESIS OF DERIVED FROM 3-CETO-CYCLOPENTENE-5-OXY

Squarylium compounds for use in display devices

PROCESSO PARA A PREPARACAO DE 4-(6"-METOXI-2"-NAFTIL)BUTAN-2-ONA

BENZYL PYRIMIDINES AND PROCESS FOR PREPARING SAME

2-HYDROXYL-4-N-PROPYL-1-TROPONE ESTER OR SALT AND APPLICATION THEREOF IN PREPARING ANTIBACTERIAL AGENT FOR ANIMALS AND GROWTH PROMOTER FOR FEED

A 2-hydroxyl-4-n-propyl-1-tropone ester or salt compound represented by formula 1 or formula 2. R1 in formula 1 represents n-heptadecyl, and L in formula 2 is sodium, potassium, calcium, magnesium, zinc, copper or manganese. The 2-hydroxyl-4-n-propyl-1-tropone ester or salt compound has high stability and safety and good antibacterial and growth promotion effects, and thus is more suitable for use as a special antibacterial agent for animals and a growth promoter for feed, and has a great application prospect in the farming industry.

POROUS SOLID ACID CATALYSTS, METHODS OF MANUFACTURING THE SAME, AND METHODS OF MANUFACTURING ORGANICS MOLECULES USING THE SAME

This invention relates to a process for synthesizing organic molecules utilizing a novel porous acid catalyst. The inventive processes are generally nucleophilic reactions employing a solid acid catalyst that has a pore size distribution having at least two different modes. The properties of the catalysts allow for relatively high product yields while at the same time provide the benefits of other solid catalysts, these benefits being manageable catalyst recycle and reduction and/or elimination of environmentally unfriendly solvents. The novel catalyst can be prepared by steam treating conventional crystalline zeolites under conditions sufficient to produce tailored pore size distributions having two or more modes of average of pore sizes, and optionally forming them into catalyst forms and/or particles. Accordingly, this invention also relates to the manufacture of the catalyst.

PROCESS FOR THE PREPARATION OF 2-HYDROXYALKYL HALOPHENONES

A process is provided for the preparation of compounds of Formula (1); wherein X1 and X2 are each independently H, Cl or F, provided that at least one of X1 and X2 is Cl or F; one of R1 and R2 is H and the other is OH; and R5 is an unsubstituted alkyl, preferably a C1-6 alkyl, group. The process comprises condensing a 2-chloroalkanoic acid with an optionally substituted benzyl alcohol to form a 2-(optionally substituted benzyloxy) alkanoic acid, converting the condensation product to the corresponding acid chloride and then either reacting the acid chloride with a compound of Formula (2) in the presence of a source of copper (I) to give a compound of Formula (3) wherein one of R3 and R4 is H and the other is optionally substituted benzyloxy; or reacting the acid chloride with a compound of the Formula (4): A----NH-----B wherein A and B independently represent substituted alkyl, alkoxy, aryl or oxyaryl groups, or are linked to form a heterocyclic ring to form an amide, and then reacting ...

Hydroquinone-ketone molecular compound and process for purifying hydroquinone using said molecular compound

The present invention relates to a novel compound which is considered to be a hydroquinone-ketone molecular compound. The invention also pertains to the method of producing such molecular compounds from hydroquinone and ketone. When the molecular compound is decomposed in the presence of water or an aqueous medium, hydroquinone can be obtained which undergoes little or no coloring even if left standing in the air for a prolonged period of time.

Heterocyclic compounds

Derivatives of acetoacetic acid, their process of preparation and their use

Novel esters useful for preparing musk extracts Novel esters of specific formulas are new. Novel esters of formulae (Ia) and (Ib) , their esters, optically active forms, tautomers, racemates, distereomer mixtures or salts are claimed: R = phenyl or 1-6C alkyl or alkoxyalkyl, where the alkoxy is a combination of an alkoxy group with an oxygen atom, e.g. (m)ethoxy, propoxy, butoxy or pentoxy. Independent claims are included for: (1) preparation of these esters and their mixtures by radically reacting an acetate of formula (II) with 1,9-decandiene; (2) preparation of 1,15-hexadecadiones by reacting the ester of (II) with 1,9-decandiene and decarboxylating; (3) preparation of muscones of formula (III) by further reacting this product in the gaseous phase to give muscones, cyclizing in a mixture with unsaturated muscone derivatives and hydrogenating to muscone.

REDUCTION APPARATUS FOR CARBON DIOXIDE GAS

PROBLEM TO BE SOLVED: To provide a reduction apparatus for a carbon dioxide gas, having a high treatment capacity of carbon dioxide gas separation. SOLUTION: This reduction apparatus for a carbon dioxide gas comprises elements consisting of an anode supporting a photocatalyst 8 constituted of titanium oxide on the surface of and in an electroconductive layer 7, a cathode supporting a photocatalyst 8 constituted of silicon carbide on the surface and in the electroconductive layer 7 and an electrolytic film 10 nipped by the anode and the cathode, and water supplied to the anode is oxidized by using photocatalytic ability of titanium oxide and carbon dioxide gas supplied to the cathode is reduced by using photocatalytic ability of silicon carbide, and the reaction of the all elements are promoted to consequently improve decomposition treatment capacity of carbon dioxide gas. COPYRIGHT: (C)2001,JPO ...

СПОСОБ ПОЛУЧЕНИЯ 3-ТРИФТОРМЕТИЛЬНЫХ ХАЛКОНОВ

Изобретение относится к улучшенному способу получения соединения формулы, где Z представляет собой необязательно замещенный фенил; Q представляет собой фенил или 1-нафталенил, каждый необязательно замещенный. Способ включает дистилляцию воды из смеси, содержащей соединение формулысоединение формулы, основание, содержащее по меньшей мере одно соединение, выбранное из группы, содержащей гидроксиды щелочноземельного металла формулы, где M представляет собой Ca, Sr или Ba, карбонаты щелочного металла формулы, где Mпредставляет собой Li, Na или K, 1,5-диазабицикло[4.3.0]нон-5-ен и 1,8-диазабицикло[5.4.0]ундец-7-ен, и апротонный растворитель, способный образовывать низкокипящий азеотроп с водой. Изобретение также относится к способу получения соединения формулы 2, к способу получения соединения формулыиз соединения формулы 1 и к соединению формулы 2. Способ позволяет получать продукт с высоким выходом. 5 н. и 15 з.п. ф-лы, 15 табл., 8 пр.

ИНГИБИТОРЫ ФОСФОДИЭСТЕРАЗЫ ТИПА-IV

Настоящее изобретение относится к соединениям структурной формулы I и их фармацевтически приемлемым солям. В структурной формуле I ! ! Х представляет собой кислород; Y представляет собой кислород; Y1, Y2, R7 и R4 представляют собой Н; X1 и Х2 выбраны независимо из группы, состоящей из водорода, алкильной группы, содержащей от 1 до 5 атомов углерода, в которой один или более атомов водорода алкильной группы могут быть замещены галогеном, арильной группой, содержащей от 6 до 10 атомов углерода или циклоалкильной группой, содержащей от 3 до 9 атомов углерода, или 5-9-членной гетероциклической группой с 2 гетероатомами, выбранными из N и О, или циклоалкильной группы, содержащей от 5 до 9 атомов углерода; значения остальных радикалов представлены в формуле изобретения. Изобретение также относится к фармацевтической композиции, обладающей свойствами селективных ингибиторов фосфодиэстеразы типа IV, содержащей терапевтически эффективное количество соединения изобретения. 2 н. и 4 з.п. ф-лы.

СПОСОБ ПОЛУЧЕНИЯ 4,4,4-ТРИХЛОР-1-(4-ХЛОРФЕНИЛ)БУТАН-1,3-ДИОНА, ОБЛАДАЮЩЕГО ПРОТИВОКАНДИДОЗНОЙ АКТИВНОСТЬЮ

FIELD: chemistry. SUBSTANCE: present invention relates to a method of producing 4,4,4-trichloro-1-(4-chlorophenyl)butane-1,3-dione of formula , having anti-Candidiasis activity. Method consists in fact that 4-chloro-1-(1,1-diethoxy)benzene in the presence of pyridine in anhydrous chloroform is cooled down to 0 °C, a solution of trichloroacetic acid chloride is added while stirring, reaction mixture is held at stirring for 10 hours, after time 2M sulfuric acid is added and stirring is carried out for 2 hours at temperature of 80 °C, the obtained mixture is separated on a separatory funnel, the organic layer is dried with sodium sulphate, after removal of solvent, the precipitated product is recrystallised, followed by extraction of the end product. Trichloroacetic acid chloride solution is pre-cooled to 0 °C before adding to reaction mixture; holding the reaction mixture while stirring for 10 hours is carried out at room temperature, without moisture access; before transfer into separating funnel mixture is cooled; separated organic layer is washed with distilled water until neutral medium reaction; filtrate obtained after drying the washed organic layer over anhydrous sodium sulphate is passed through a layer of silica gel; evaporated; formed precipitate of compound is recrystallised twice from ethanol. EFFECT: disclosed method enables to obtain an end product which does not contain undesirable impurities, with output of 88 %. 5 cl, 2 tbl, 2 ex РОССИЙСКАЯ ФЕДЕРАЦИЯ (19) RU (11) (13) 2 690 009 C1 (51) МПК C07C 45/61 (2006.01) C07C 45/78 (2006.01) C07C 49/80 (2006.01) ФЕДЕРАЛЬНАЯ СЛУЖБА ПО ИНТЕЛЛЕКТУАЛЬНОЙ СОБСТВЕННОСТИ (12) ОПИСАНИЕ ИЗОБРЕТЕНИЯ К ПАТЕНТУ (52) СПК C07C 45/61 (2019.02); C07C 45/78 (2019.02) (21)(22) Заявка: 2018104421, 06.02.2018 (24) Дата начала отсчета срока действия патента: 30.05.2019 Приоритет(ы): (22) Дата подачи заявки: 06.02.2018 (45) Опубликовано: 30.05.2019 Бюл. № 16 2 6 9 0 0 0 9 R U (56) Список документов, цитированных в отчете о поиске: RU ...

СОЕДИНЕНИЯ АЗОЛА, СПОСОБЫ ИХ ПОЛУЧЕНИЯ, ПРОМЕЖУТОЧНЫЕ СОЕДИНЕНИЯ, СПОСОБЫ ИХ ПОЛУЧЕНИЯ, ФАРМАЦЕВТИЧЕСКАЯ КОМПОЗИЦИЯ, ОБЛАДАЮЩАЯ ПРОТИВОГРИБКОВОЙ АКТИВНОСТЬЮ

Описываются новые соединения азола общей формулы I, где значения А, R1 - R3, W, X, Y, Z, m указаны в п.1 формулы, которые проявляют противогрибковую активность и могут быть использованы при лечении дерматомикоза, висцеромикоза. Описывается также способ их получения, промежуточные соединения, а также фармацевтическая композиция, обладающая противогрибковой активностью. 26 с. и 5 з.п.ф-лы, 6 табл.

СПОСОБ ПОЛУЧЕНИЯ 3,5-ДИАЛКИЛ-4-ОКСИБЕНЗИЛЗАМЕЩЕННЫХ БЕТА-ДИКАРБОНИЛЬНЫХ СОЕДИНЕНИЙ (ВАРИАНТЫ)

... 1. Способ получения 3,5-диалкил-4-оксибензил-замещенных β-дикарбонильных соединений, включающий взаимодействие β-дикарбонильного соединения с алкилирующим агентом в присутствии органического, растворителя в щелочной среде, отличающийся тем, что в качестве алкилирующего агента используют N, N-замещенный-3,5-диалкил-4-оксибензилдитиокарбамидат. 2. Способ получения 3, 5-диалкил-4-оксибензил-замещенных β-дикарбонильных соединений, включающий взаимодействие β-дикарбонильного соединения с алкилирующим агентом в присутствии органического растворителя в щелочной среде, отличающийся тем, что в качестве алкилирующего агента используют N, N-диалкил-(3,5-диалкил-4-оксибензил)-амин.

NEW ROUTE TO SYNTHETIC ANALOGUES OF ROCAGLAMIDE AND AGLAFOLINE USING CASCADE TRANSFORMATIONS INITIATED BY OXY-COPE REARRANGEMENT OF BIS-ALKYNES

A method for preparing a cyclobutene compound or a cyclopentenone is provided. The method comprises contacting an α,β-diketone with a metal acetylide at a temperature below 0° C. to thereby form a reaction mixture comprising a bis-alkyne precursor. The bis-alkyne precursor rearranges into a bis-allenic intermediate, which undergoes further rearrangement into the cyclobutene compound or the cyclopentenone compound as the temperature of the reaction mixture increases from below 0° C. to above 0° C. 1. A method of preparing a cyclobutene compound , the method comprising:contacting an α,β-diketone with a metal acetylide at a temperature below 0° C. to thereby form a reaction mixture comprising a bis-alkyne precursor;wherein the bis-alkyne precursor rearranges into a bis-allenic intermediate, which undergoes further rearrangement into the cyclobutene compound as the temperature of the reaction mixture increases from below 0° C. to above 0° C.2. The method of wherein the α claim 1 ,β-diketone and the metal acetylide are contacted at a temperature below about −50° C.3. The method of wherein the rearrangement occurs as the temperature of the reaction mixture increases from about −78° C. to room temperature.4. The method of wherein the α claim 1 ,β-diketone is contacted with the metal acetylide at a molar ratio of metal acetylide to α claim 1 ,β-diketone of at least 1.9:1.6. The method of wherein the moiety comprising the silyl functional group is selected from the group consisting of trimethylsilyl claim 5 , triethylsilyl claim 5 , tri-isopropylsilyl claim 5 , and combinations thereof.8. The method of wherein the moiety comprising the silyl functional group is selected from the group consisting of trimethylsilyl claim 7 , triethylsilyl claim 7 , tri-isopropylsilyl claim 7 , and combinations thereof.13. The method of wherein the moiety comprising the silyl functional group is selected from the group consisting of trimethylsilyl claim 12 , triethylsilyl claim 12 , tri- ...

Protected Aldehydes For Use As Intermediates In Chemical Syntheses, And Processes For Their Preparation

A para-methoxy protected benzaldehyde useful in preparation of treprostinil, and of formula: (Formula (1)) is prepared by subjecting to Claisen re-arrangement a substituted benzaldehyde of formula (1a): (Formula (Ia)) to form the m-hydroxy-substituted benzaldehyde of formula (1b): (Formula (Ib)) and then reacting compound (1b) with a p-methoxybenzyl (PMB) compound to form a PMB-substituted benzaldehyde of formula (1). 2. The process of wherein the oxyalkene-substituted benzaldehyde of formula (Ia) is prepared by reaction of the m-hydroxybenzaldehyde with an allyl halide.3. The process of any one of or wherein Step a) is performed in an organic solvent.4. The process of wherein the organic solvent is an inert claim 3 , high boiling hydrocarbon or ether claim 3 , or a mixture thereof.5. The process of wherein the organic solvent is decalin.6. The process of wherein the organic solvent is decalin claim 4 , toluene mixture. This invention relates to chemical synthesis of aldehyde compounds, useful as intermediates in preparation of pharmaceutically active prostacyclins. More specifically, it relates to synthesis of a novel, protected aryl aldehyde which can be used in the synthesis of the pharmaceutically active prostacyclin known as treprostinil, using a modified Claisen re-arrangement reaction.A Claisen re-arrangement is a highly stereoselective [3,3]-sigmatropic re-arrangement of allyl ethers or allyl aryl ethers, to yield γ, δ-unsaturated carbonyl compounds or α-allyl substituted phenols, respectively. U.S. Pat. Nos. 6,700,025 and 6,809,223 describe the Claisen re-arrangement reactions of substituted allyl aryl ethers such as 3-allylether benzaldehyde 3, to produce 2-allyl-3-hydroxy benzaldehyde, thus:As described in these patents, the reaction is conducted neat, at 150° C. for 41 hours, followed by a series of purifications to yield compound 4.Aromatic Claisen re-arrangements conducted neat are known to be dangerously reactive, with the potential of producing ...

INTERMEDIATES FOR THE PREPARATION OF BETA-SANTALOL

The present invention concerns a process for the preparation of a compound of formula (I) in the form of any one of its stereoisomers or mixtures thereof, and wherein the dotted line may represents an additional bond and Rrepresents a hydrogen atom or a Si(R)or (R)COH group, each Rrepresenting Calkyl group or a phenyl group. The invention concerns also the compound (I) as well as its use for the synthesis of β-santalol or of derivatives thereof. 3. A compound according to , wherein X may represent a halogen atom or a sulfonate group as defined in .4. A compound according to claim 1 , wherein Rrepresents a hydrogen atom or a Si(R) claim 1 , each Rrepresenting a Calkyl group or a phenyl group.5. A compound according to claim 1 , wherein said compound is in the form of a mixture of stereoisomers comprising more than 50% (w/w) of:the (1RS,4SR) or the (1RS,2SR,4SR) diastereoisomer, when the dotted line represents a single bond; orthe (1RS,4SR) or the (1RS,2RS,4SR) diastereoisomer, when the dotted line represents a double bond.6. A compound according to claim 1 , wherein said compound is in the form of a mixture of stereoisomers comprising more than 50% (w/w) ofthe (1S,4R) or (1S,2R,4R) enantiomer, when the dotted line represents a single bond; orthe (1R,4S) or (1R,2R,4S) enantiomer, when the dotted line represents a double bond.7. A process for the preparation of a compound of formula (I) claim 1 , as defined in claim 1 , comprising the following steps:{'claim-ref': {'@idref': 'CLM-00002', 'claim 2'}, 'sub': 'a', 'a) reacting a compound of formula (II), as defined in , with a base having a pKabove 16, preferably comprised between 16 and 30;'}{'sup': a', 'a, 'b) optionally, when Ris not a hydrogen atom, treating the compound obtained in step a) with a suitable base or a fluorine salt to obtain compound (I) wherein Ris hydrogen atom.'} The present invention relates to the field of organic synthesis and more specifically it concerns a process for the preparation of a ...

METHOD FOR SYNTHESIZING BETA-DICARBONYL COMPOUNDS

A method for synthesizing beta-dicarbonyl compounds, particularly beta-diketones, from at least two carbonyl compounds, such as esters and ketones, in the presence of a strong base or a mixture of strong bases by Claisen condensation with a titer of greater than 95%. The method includes providing a synthesis reactor on which a separation column, provided with a condenser and with at least one microwave generator, is mounted; feeding a first carbonyl compound and the strong base into the synthesis reactor; heating the reactor and starting up the condenser; starting up the microwave generator(s); when the mixture is brought to a boil at total flux, feeding the second carbonyl compound into the reactor; and after a waiting time, stopping the reactor and acidifying and washing the reaction mixture.) 111-. (canceled)13. The process of claim 12 , wherein the reactor includes at least one microwave source directly mounted inside the reactor and an external microwave source connected to the reactor via a wave guide to conduct the microwaves into the reaction mixture.14. The process of claim 12 , wherein the reactor includes an external recirculating loop having a pump and a microwave source.15. The process of claim 12 , wherein the carbonyl compounds comprises at least one ketone and at least one ester.16. The process of claim 15 , wherein the ketone is in molar excess compared with the ester.17. The process of claim 12 , wherein the conjugate acid of the strong base is volatile in the conditions of the reaction.18. The process of claim 17 , wherein the strong base is an alcoholate.19. The process of claim 12 , wherein the reaction temperature is between 60-180° C.20. The process of claim 12 , wherein the reaction is conducted in the absence of any solvent.21. The process of claim 12 , wherein the reaction is conducted in the presence of one of a pure solvent and a mixed solvent.22. The process of claim 12 , wherein a gentle flow of nitrogen gas is maintained in the reactor ...

Organo-cascade catalysis: one-pot production of chemical libraries

A method for production of a chemical library is provided, where the method involves: reacting, in a single vessel, a) a plurality, x, of aldehydes and/or ketones; and b) either (i) a plurality, y, of nucleophiles, (ii) a plurality, z, of electrophiles or both (i) and (ii); in the presence of c) a cascade catalyst capable of catalyzing reaction between said plurality of aldehydes and/or ketones and said plurality of nucleophiles, said plurality of electrophiles or both; to obtain a mixture of x-y β-nucleophile substituted aldehydes and/or ketones, x•z α-electrophile substituted aldehydes and/or ketones or x•y•z β-nucleophile substituted, α-electrophile substituted aldehydes and/or ketones; and the chemical libraries thus produced.

CONTINUOUS PRODUCTION OF METHYL PENTENONE USING CATION EXCHANGE RESIN IN A FIXED BED REACTOR

Provided herein is a method for producing methyl pentenone (MPO) in high yield in a continuous mode in a fixed bed reactor having a plurality of sidewall injecting ports by reacting excess methyl ethyl ketone (MEK) with acetaldehyde in presence of a cation exchange resin catalyst, wherein the acetaldehyde is injected from the plurality of sidewall injecting ports of the reactor. The method is also effective in reducing the complete consumption of the catalyst during the course of the reaction. 1. A method for producing methyl pentenone (MPO) in a continuous mode in high yield , the method comprising a reaction between methyl ethyl ketone (MEK) and acetaldehyde in presence of a heterogeneous catalyst in a fixed bed reactor having a plurality of sidewall injecting ports , wherein MEK is fed in a bed of the heterogeneous catalyst in the reactor and acetaldehyde is injected from the plurality of sidewall injecting ports and wherein the concentration of acetaldehyde to methyl ethyl ketone is from 1:3 to 1:18 (feed molar ratio).2. The method as claimed in claim 1 , wherein the heterogeneous catalyst is a cation exchange resin catalyst.3. The method as claimed in claim 2 , wherein the cation exchange resin catalyst is selected from the group consisting of Polystyrene sulphonated cation resin claim 2 , a Polymeric resin claim 2 , a solid catalyst supported on clay claim 2 , a solid acid catalyst supported on polymeric resin claim 2 , solid aluminophosphate claim 2 , Amberlyst-15 claim 2 , Amberlyst-35 claim 2 , Langson dry Lewatit K2620 catalyst claim 2 , Dry NKC claim 2 , Dry purolite claim 2 , Zinc acetate claim 2 , zinc acetate dehydrate claim 2 , and aluminium phosphate.4. The method as claimed in claim 1 , wherein the reaction takes place at a temperature of 343-363 K.5. The method as claimed in claim 1 , wherein the reaction takes place at a residence time of 295-345 min.6. The method as claimed in claim 1 , wherein injection of acetaldehyde from the plurality of ...

METHODS OF MAKING MULTICYCLIC COMPOUNDS USING MULTICOMPONENT/TANDEM REACTION SEQUENCES

Disclosed herein are embodiments of multicyclic compounds and methods of making such compounds. The disclosed methods reduce step-counts in the synthesis of complex targets, while reducing costs and waste streams. 1. A method , comprising combining an alkyne-containing compound comprising a carbonyl functional group , a diene , and a Lewis acid to form a multicyclic compound comprising one or more fused ring systems.3. The method of claim 1 , wherein the alkyne-containing compound is a diynone.4. The method of claim 3 , wherein the diynone comprises two terminal functional groups that facilitate regiochemical control.6. The method of claim 5 , wherein each Rindependently is selected from aryl claim 5 , aliphatic claim 5 , heteroaryl claim 5 , heteroaliphatic claim 5 , or —Si(R) claim 5 , wherein each R independently is selected from hydrogen claim 5 , aliphatic claim 5 , heteroaliphatic claim 5 , aryl claim 5 , or heteroaryl.7. The method of claim 4 , wherein each Rindependently is selected from phenyl; pyridinyl; thiophenyl; naphthyl; meta- claim 4 , ortho- claim 4 , or para-methoxyphenyl; meta- claim 4 , ortho- claim 4 , or para-trifluoromethylphenyl; meta- claim 4 , ortho- claim 4 , or para-bromophenyl; meta- claim 4 , ortho- claim 4 , or para-fluorophenyl; meta- claim 4 , ortho- claim 4 , or para-chlorophenyl; meta- claim 4 , ortho- claim 4 , or para-iodophenyl; cyclopropyl; cyclobutyl; cyclopentyl; cyclohexyl; methyl; ethyl; propyl; butyl; pentyl; or t-butyl.10. The method of claim 9 , wherein Ris selected from hydrogen claim 9 , methyl claim 9 , ethyl claim 9 , propyl claim 9 , butyl claim 9 , pentyl claim 9 , phenyl claim 9 , methoxy claim 9 , ethoxy claim 9 , propoxy claim 9 , —Si(Me) claim 9 , —Si(Et) claim 9 , or —Si(iPr).11. The method of claim 9 , wherein Ris selected from phenyl; pyridinyl; meta- claim 9 , ortho- claim 9 , or para-methoxyphenyl; meta- claim 9 , ortho- claim 9 , or para-trifluoromethylphenyl; meta- claim 9 , ortho- claim 9 , or para- ...

CATALYTIC CYCLE FOR PRODUCTION OF 1,1-DISUBSTITUTED ALKENES

The present teachings disclose contacting an amine salt catalyst with a dicarbonyl compound having an alkylene group between the carbonyl group; adding formaldehyde, paraformaldehyde, or formalin in an amount of about 2:1 to about 3:1 moles of formaldehyde to moles of the dicarbonyl compound to form a mixture; and refluxing the mixture. The process forms a carbonyl-substituted alkene. The process may be performed in the absence of a solvent. The process may form methylene malonates, methylene dimalonates, methylene keto malonamides, methylene diketones, methylene keto esters, and the like. 2. The process of claim 1 , wherein the process is a Mannich-type reaction.3. The process of claim 1 , wherein the formaldehyde claim 1 , paraformaldehyde claim 1 , formalin or trioxane is added in an amount of 2.0 to 2.1 equivalents.4. The process of claim 1 , wherein the diester or ketoester compound is a hydrocarbyl malonate claim 1 , where the hydrocarbyl group is an alkyl claim 1 , cycloalkyl claim 1 , polyether group.5. The process of claim 4 , wherein the diester or ketoester compound is selected from diethyl malonate; dicyclohexyl malonate; or ethyl cyclohexyl malonate.6. The process of claim 1 , wherein the amine salt catalyst is prepared by reacting an acid with a base claim 1 , and wherein the acid has a Bronsted acidity of 2 to −6.7. The process of claim 6 , wherein the base is a sterically hindered ammonium cation.8. The process of claim 6 , wherein the base is a secondary ammonium cation.9. The process of claim 6 , wherein the acid has a pKa of about 2 to about 6.10. The process of claim 6 , wherein the acid is selected from trifluoroacetic acid claim 6 , sulfuric acid claim 6 , methanesulfonic acid claim 6 , or acetic acid.11. The process of claim 1 , wherein the amine salt catalyst is diisopropylammonium trifluoroacetate claim 1 , diisopropylammonium acetate claim 1 , or diisopropylammonium methanesulfonate.12. The process of claim 1 , wherein the amine salt ...

PROCESS FOR THE IN SITU ACTIVATION OF ZINC METAL

A non-carcinogenic process for the activation of zinc metal in a medium polarity solvent, wherein said zinc metal is activated by the reaction thereof with a halogen and a lithium compound selected from lithium halides and lithium pseudohalides, the use of said activated zinc metal for the preparation of an organozinc halide of formula R—ZnX, and a process for the preparation of compounds obtainable by the reaction of said organozinc halide of formula R—ZnX with compounds having functionality enabling them to react with said organozinc halide. 1. A process for the activation of zinc metal in a medium polarity solvent having a low nucleophilicity , wherein said zinc metal is activated by the reaction thereof with a halogen and a lithium compound selected from lithium halides and lithium pseudohalides.2. A process according to claim 1 , wherein said zinc metal is first mixed with said lithium compound claim 1 , before the addition of said solvent to the resulting product and then finally the addition of said halogen.3. A process according to claim 2 , wherein the mixture resulting from the addition of said lithium compound to said zinc metal is dried before the addition of said solvent.4. A process according to claim 2 , wherein the mixture produced after the addition of said halogen is heated.5. A process according to claim 1 , wherein the activation of the zinc metal takes place in a medium polarity solvent that does not react with any reagents or intermediates in the process.6. A process according to claim 5 , wherein the solvent is selected from the group consisting of tetrahydrofuran claim 5 , diethyl ether claim 5 , any other symmetric or asymmetric claim 5 , cyclic or acyclic claim 5 , substituted or unsubstituted dialkylether claim 5 , dichloromethane claim 5 , and ethyl acetate claim 5 , with the proviso that the solvent chosen must not react with or interfere in an unwanted manner with any subsequent reagent or chemical process.7. A process according to ...

Deuterated 1-piperazino-3-phenyl indanes for treatment of schizophrenia

The present invention relates to deuterated 1-piperazino-3-phenyl-indanes and salts thereof with activity at dopamine receptors Dand Das well as the 5HTreceptors in the central nervous system, to medicaments comprising such compounds as active ingredients, to the use of such compounds in the treatment of diseases in the central nervous system, and to methods of treatment comprising administration of such compounds. 3. The process of claim 1 , wherein the compound of formula (XV) is obtained in 96% enantomeric excess.5. The process of claim 4 , wherein (1R claim 4 ,3S)-(IV)-tartrate is crystallized from ethanol.6. The process of claim 5 , wherein racemic trans-1-(6-chloro-3-phenyl(d)-indan-1-yl)-1(d) claim 5 , 2 claim 5 ,2-trimethyl piperazine is generated from the corresponding succinate salt thereof.7. The process of claim 6 , wherein racemic trans-1-(6-chloro-3-phenyl(d)-indan-1-yl)-1(d) claim 6 , 2 claim 6 ,2-trimethyl piperazine succinate is generated from the maleate salt of trans-1-(6-chloro-3-phenyl(d)-indan-1-yl)-3 claim 6 ,3-dimethyl piperazine.8. A product prepared by the process of .9. A product prepared by the process of .10. A polymorph of the hydrogen tartrate salt of compound (IV) having the XRPD pattern as shown in .11. The polymorph of claim 10 , wherein the polymorph is a solvent free crystal form. This application is a continuation of U.S. patent application Ser. No. 13/924,849, filed Jun. 24, 2013 as a continuation of U.S. patent application Ser. No. 13/527,364, filed Jun. 19, 2012 and issued as U.S. Pat. No. 8,575,174 on Nov. 5, 2013, which claims priority to U.S. Provisional Application Nos. 61/498,651, filed on Jun. 20, 2011, and 61/537,103, filed on Sep. 21, 2011, the entirety of each of which is incorporated herein by reference.All patents, patent applications and publications cited herein are hereby incorporated by reference in their entirety. The disclosures of these publications in their entireties are hereby incorporated by reference ...

Method for producing hexafluoroacetone monohydrate

Synthetic method for improving yield of 5-chloro-1-indanone

本发明提供一种提高5‑氯‑1‑茚酮收率的合成方法，属于有机合成的技术领域。制备方法为：以3,4’‑二氯苯丙酮为原料，加入非质子酸催化剂后加热至熔融状态，然后加入相转移催化剂进行反应。所述非质子酸催化剂为AlCl 3 、ZnCl 2 、InCl 3 、TiCl 4 、BF 3 、Fe(CF 3 SO 3 ) 3 、Fe(CF 3 SO 3 ) 2 、γ‑氧化铝中的一种；所述相转移催化剂为四丁基溴化铵、四丁基氯化铵、三辛基甲基氯化铵、苄基三乙基氯化铵、十二烷基三甲基氯化铵、十八冠六、十五冠五、聚乙二醇400、聚乙二醇600、聚乙二醇800中的一种。本发明通过加入相转移催化剂，明显的提高了傅克反应的选择性，降低了副反应的发生，提高了反应收率。

Dihydroxybutanones

Dihydroxybutanones having the general formula WHEREIN R1 and R2 are the same or different alkyl groups of from one to 10 carbon atoms are prepared by selective hydrogenation of hydroxy furanones having the formula WHEREIN R1 and R2 are as previously described. The selective hydrogenation of the starting material is effected at a temperature in the range of between 80* to 115* C. and a pressure of between 500 to 4,000 psig. in the presence of a Raney nickel catalyst. The dihydroxybutanones are useful as intermediates for preparation of commercially useful products such as polyols, solvent esters, polyesters and polyurethane products.

Preparation method of 3, 5-dihalo-trifluoro-acetophenone and derivatives thereof

本申请涉及化工制药的技术领域，尤其是涉及一种3,5‑二卤三氟苯乙酮及其衍生物的制备方法，以3‑卤素‑4‑硝基三氟苯乙酮为原料，经过还原反应、卤代反应和氨基取代反应，最终得到3,5‑二卤三氟苯乙酮的衍生物，其原料便宜易得，工艺简单，条件温和，具有大规模生产的前景，具有较好的经济效应。

Polyether ketone, its monomer and its phenolate

本发明涉及聚醚酮、其单体以及其酚盐。本发明涉及一种用于制备4-氯-4′-羟基二苯甲酮的碱金属盐的方法，包括以下步骤：(a)通过包括在减压下蒸馏包含4-氯-4′-羟基二苯甲酮和选自二苯砜、二亚苯砜、二苯甲酮以及二氯二苯甲酮的溶剂的液体的方法来制备纯化的4-氯-4′-羟基二苯甲酮，然后(b)通过纯化的4-氯-4′-羟基二苯甲酮与化学计量过量的至少一种碱金属碱反应来制备由此纯化的4-氯-4′-羟基二苯甲酮的碱金属盐。还描述了一种使用碱金属盐来生产具有高特性粘度和改善的机械和热性能的PEK的聚合方法。

Polyether ketone its monomer and its phenolate

(a) 4-chloro-4 ' -hydroxybenzophenone, and 4-chloro-4 ' -hydroxybenzophenone and a solvent selected from diphenylsulfone, diphenylene sulfone, benzophenone and dichlorobenzophenone -Chloro-4 '-hydroxybenzophenone; And then (b) an alkali metal salt of 4-chloro-4'-hydroxybenzophenone, purified by the reaction of purified 4-chloro-4'-hydroxybenzophenone with at least one stoichiometric excess of alkali metal base, Chloro-4 &apos; -hydroxybenzophenone. &Lt; / RTI &gt; There is also a description of a polymerization process using alkali metal salts to produce PEK having high intrinsic viscosity and improved mechanical and thermal properties.

Method for preparing keto-isophorone

본 발명은 반응용매, 염기 및 건조제 존재 하에서 CuCl 2 나 CuCl을 단독 또는 CuI와 혼합한 촉매를 사용하고, 산소 또는 공기를 주입하는 산화반응을 통하여 β-이소포론으로부터 케토-이소포론을 제조하고, 상기 반응의 부산물인 4-히드록시 이소포론을 물로 세척한 다음 유기층으로부터 케토-이소포론을 분리하는 고수율 및 고순도 케토-이소포론의 제조방법에 관한 것이다. 본 발명에 따른 CuCl 2 나 CuCl을 단독 또는 CuI와 혼합한 촉매의 사용은 반응 부산물로서 4-히드록시 이소포론만을 생성하며, 이는 물로 세척하여 완전히 제거됨으로써 고순도 케토-이소포론을 경제적으로 제조할 수 있다. The present invention provides a keto-isophorone from β-isophorone through an oxidation reaction in which oxygen or air is injected using a catalyst in which CuCl 2 or CuCl is mixed alone or with CuI in the presence of a reaction solvent, a base and a desiccant, 4-hydroxy isophorone, which is a byproduct of the reaction, is washed with water, and then a high yield and high purity method for preparing keto-isophorone isolating keto-isophorone from an organic layer. The use of a catalyst comprising CuCl 2 or CuCl alone or in combination with CuI according to the present invention produces only 4-hydroxy isophorone as reaction byproduct, which can be economically prepared with high purity keto-isophorone by washing it off completely with water. have. β-이소포론, 케토-이소포론, CuCl2/CuCl, CuI, 4-히드록시 이소포론 β-isophorone, keto-isophorone, CuCl 2 / CuCl, CuI, 4-hydroxy isophorone

Oxime-based dynamically repairable polyurethane and preparation method thereof

本发明提供一种多官能团肟及其制备方法、和一种基于肟的新型动态可修复聚氨酯及其制备方法，所述肟是一种具有高反应活性的有机物，其与异氰酸酯在室温、无催化剂的条件下就可制备得到本发明所述的聚氨酯。值得注意的是，肟通常可由羰基化合物(醛或酮)与羟胺在温和的条件下反应获得，该过程是一种原子经济的、高产率的、简便的反应。所述热固性肟基聚氨酯切成小碎块，在90～120℃，1～100MPa的条件下可再次热压成型，所得热固性聚氨酯基本恢复原始的机械性能；所述聚氨酯在室温下，无需催化剂的条件下就可以实现反应的进行；所述制备方法简单，制备过程原料来源广泛，生产成本低，具有大规模工业化生产的前景。

Preparation method of terbutaline sulfate

本发明公开了一种硫酸特布他林的制备方法，该方法采用3,5‑二羟基苯乙酮为起始原料，先经苄基保护后得到3,5‑二苄氧基苯乙酮，3,5‑二苄氧基苯乙酮经过溴化铜溴代、DMSO氧化得到3,5‑二苄氧基苯乙酮醛，然后与叔丁胺还原胺化生成1‑[3,5‑二(苄氧基)苯基]‑2‑(叔丁基氨基)乙醇，最后经过氢化脱苄和硫酸成盐得到硫酸特布他林。与现有技术相比，本发明所使用的原辅料均价廉易得，避免使用高危剧毒试剂，没有高温高压反应，操作简便，反应条件温和，解决了现有工艺中步骤长收率低，具有安全隐患等缺点。

Synthetic method of ultraviolet ray absorber BP-2

本发明公开了一种紫外线吸收剂BP-2的合成方法，主要包括下述工艺步骤：①酯化反应：向反应釜中投入间苯二酚和氯仿，溶解后滴加乙酰氯，反应2-2.5h，得醋酸二酚酯；②酰化反应：向反应釜加入酯化产物醋酸二酚酯及二氯乙烷、N，N-二甲基甲酰胺和无水三氯化铝，再缓慢滴加固体光气，反应完毕，蒸馏回收溶剂，釜内固体剩余物冷却至室温；③水解反应：以10%稀盐酸溶解釜内的固体剩余物，升温水解反应，冷却，静置，固体析出，抽滤、水洗，得到粗产品；粗产品精制，得到BP-2；本发明方法工艺简单、条件温和、生产成本低，适合工业化生产。

Preparation method of gem-difluoroolefin compound

本发明公开了一种偕二氟烯烃化合物的制备方法，将三氟甲基烯烃化合物在二苯基氧膦、碳酸铯的作用下，于溶剂中进行加氢脱氟反应，得到偕二氟烯烃化合物。本发明反应条件温和，官能团耐受性好，具有良好的区域选择性。

Process to produce prostratin and structural or functional analogs thereof

This invention concerns a process to convert a hydroxyl group (bold in R 3 C—OH) in a tigliane-type compound to a hydrogen (bold in R 3 C—H) to obtain deoxytigliane-type compounds or structural or functional analogs thereof. The process has wide application particularly to produce specific biologically active compounds in quantity for use as pharmaceuticals. In particular the process can be used to convert phorbol to a 12-deoxytigliane (prostrating which is a therapeutic lead for the treatment of AIDS. New compositions of matter are also disclosed.

Polyether ketone, its monomer and its phenolate

A process for the preparation of an alkali metal salt of 4-chloro-4′-hydroxy benzophenone including the steps of (a) preparing purified 4-chloro-4′-hydroxy benzophenone by a process including distilling under reduced pressure a liquid containing 4-chloro-4′-hydroxy benzophenone and a solvent selected from diphenyl sulphone, diphenylene sulphone, benzophenone and dichlorobenzophenone, and then (b) preparing the alkali metal salt of thus purified 4-chloro-4′-hydroxy benzophenone by the reaction of the purified 4-chloro-4′-hydroxy benzophenone with a stoichiometric excess of at least one alkali metal base. There is also described a polymerization process using the alkali metal salt to yield PEK with high inherent viscosity and improved mechanical and thermal properties.

A kind of preparation method of dezocine key intermediate

本发明公开了一种地佐辛关键中间体的制备方法，以7‑甲氧基‑2‑萘满酮为原料，首先在苄位甲基化，再在羰基的邻位进行烷基化，可以通过分步合成、两步法和一锅法三种策略进行制备。本发明的地佐辛关键中间体的制备方法，合成路线简捷、步骤少，产率高，操作简单，大大缩短了合成周期；反应条件温和，提高了工艺的安全性；原料成本低；便于产业化。本发明所涉及的简捷合成方法在很大程度上降低制剂的成本，进而降低患者的用量成本，也会在一定程度上减少国家的社保开支，产生一定的社会和经济效益。

Polyether ketone, its monomer and its phenolate

A process for the preparation of an alkali metal salt of 4-chloro-4'-hydroxy benzophenone comprising of the steps of (a) preparing purified 4-chloro-4'-hydroxy benzophenone by a process comprising distilling under reduced pressure a liquid containing 4-chloro-4'-hydroxy benzophenone and a solvent selected from diphenyl sulphone, diphenylene sulphone, benzophenone and dichlorobenzophenone, and then (b) preparing the alkali metal salt of thus purifed 4-chloro-4'-hydroxy benzophenone by the reaction of the purified 4-chloro-4'-hydroxy benzophenone with a stoichiometric excess of at least one alkali metal base. There is also described a polymerization process using the alkali metal salt to yield PEK with high inherent viscosity and improved mechanical and thermal properties.

Polyether ketone, its monomer and its phenolate

一种用于制备4－氯－4′－羟基二苯甲酮的碱金属盐的方法，包括以下步骤：(a)通过包括在减压下蒸馏包含4－氯－4′－羟基二苯甲酮和选自二苯砜、二亚苯砜、二苯甲酮以及二氯二苯甲酮的溶剂的液体的方法来制备纯化的4－氯－4′－羟基二苯甲酮，然后(b)通过纯化的4－氯－4′－羟基二苯甲酮与化学计量过量的至少一种碱金属碱反应来制备由此纯化的4－氯－4′－羟基二苯甲酮的碱金属盐。还描述了一种使用碱金属盐来生产具有高特性粘度和改善的机械和热性能的PEK的聚合方法。

Method for preparing free gossypol by using gossypol acetate as raw material

本发明涉及一种以醋酸棉酚为原料制备游离棉酚的方法，该方法通过超声破坏醋酸棉酚中醋酸和棉酚之间的分子间氢键，然后让醋酸进入水溶液或饱和食盐水溶液中，实现游离棉酚和醋酸的分离，将粗制游离棉酚进行重结晶得到高纯度的游离棉酚，整个制备过程在室温下进行，并且制备时间短，有效避免棉酚结构氧化和各种异构体之间的转换，该方法原料成本低，工艺流程短，重复性好，纯度高、安全性高，时间短，效率高，本发明具有一定的经济价值和实用价值。

Preparation method of 3, 5-dihalo trifluoro acetophenone and its derivative

本申请涉及化工制药的技术领域，尤其是涉及一种3,5‑二卤三氟苯乙酮及其衍生物的制备方法，以3‑卤素‑4‑硝基三氟苯乙酮为原料，经过还原反应、卤代反应和氨基取代反应，最终得到3,5‑二卤三氟苯乙酮的衍生物，其原料便宜易得，工艺简单，条件温和，具有大规模生产的前景，具有较好的经济效应。

A kind of preparation process of acetylacetonate

本发明公开了一种乙酰丙酮盐的制备工艺，采用金属化合物与乙酰丙酮通过加压方式配合催化剂的作用，直接促使乙酰丙酮与金属化合物完全反应制得乙酰丙酮盐，通过对压力的控制使反应体系内的物料流动性增加，无需特殊处理和其他大量溶液作为分散介质，也无需强力剪切即可让物料充分混合反应，反应均匀且彻底，得到产品质量更加均匀稳定，且本发明的技术方案反应速度快、反应条件温和易于控制，过程无无废液产生，消除了对环境的污染，降低了产品的成本，并且原料的工艺损失少，有利于提高产品的收率，以乙酰丙酮计，成品乙酰丙酮盐收率在95％以上。

2,4-diethylocta-2,6-dienal and its use as aroma chemical

The present invention relates to 2,4-diethylocta-2,6-dienal and a method of preparing same, to the use of 2,4-diethylocta-2,6-dienal as aroma chemical; to the use of 2,4-diethylocta-2,6- dienal for preparing an aroma chemical composition or for modifying the aroma character of an aroma chemical composition; to an aroma chemical composition containing 2,4- diethylocta-2,6-dienal; and to a method of preparing an aromatized composition or for modifying the aroma character of an aromatized composition.

The method for preparing (4S)-or (4R) -3,4- dihydroxy -2,6,6- 3-methyl cyclohexanol -2- ketenes

本发明涉及制备3,4‑二羟基‑2,6,6‑三甲基环己‑2‑烯酮对映体之一的新方法，以及制备(3S，3'S)‑虾青素的方法，该方法包括：提供3,4‑二羟基‑2,6,6‑三甲基环己‑2‑烯酮的(4S)‑对映体的步骤。

Method for producing polyether ketone which is monomer as well as phenolate

【課題】 高い特有粘度を有し優れた力学特性と熱安定性を有するポリエーテルケトン（ＰＥＫ）の改良された工業的な製造方法を提供する。 【解決手段】 本発明のポリエーテルケトンの製造方法は、４−クロロ−４’−ヒドロキシベンゾフェノンと４−クロロ−４’−ヒドロキシベンゾフェノンよりも沸点が低くてその低い沸点にて熱安定性のある相溶性溶媒とを含む液体を減圧下で蒸留することで４−クロロ−４’−ヒドロキシベンゾフェノンを精製する段階（ａ）と、精製した４−クロロ−４’−ヒドロキシベンゾフェノンと化学量論的に余剰な少なくとも１種のアルカリ金属塩基との反応によって４−クロロ−４’−ヒドロキシベンゾフェノンのアルカリ金属化合物を調合する段階（ｂ）からなる。 【選択図】 なし

Preparation method of 2-alkoxy-2-cyclopentene-1-ketone

本发明公开了一种制备2‑烷氧基‑2‑环戊烯‑1‑酮的方法，具体为以环戊酮和脂肪醇为反应底物，在当量碘和铜盐存在下，经由碘化、取代、氧化及加成消除的串联反应得到2‑烷氧基‑2‑环戊烯‑1‑酮。环戊酮的化学结构通式为 ，醇的化学结构通式为R 2 OH，铜盐选自乙酸铜、碘化亚铜、单质铜和氧化铜中的一种。本发明公开的制备方法具有原料易得、底物范围广、操作简单方便和绿色安全等优点。

一种5-氯-1-茚酮的制备方法

本发明涉及化学合成领域，具体涉及一种5‑氯‑1‑茚酮的制备方法。主要特点在于烷基化反应过程中加入相转移催化剂，相转移催化剂的作用是降低了烷基化反应温度，提高产品合成收率；更重要的是提高了烷基化反应体系的流动性，相对低温下进行三氯化铝水解处理过程中可实现自动化匀速滴加，操作方便，节省人力物力，有利于工业化生产。

Organo-cascade catalysis: one-pot production of chemical libraries

一种维生素b1中间体的绿色合成方法

本发明公开了一种维生素B1中间体的绿色合成方法，在催化剂存在下使α‑乙酰基‑γ‑丁内酯在有氧条件下、在溶剂中反应，生成α‑羟基乙酰基‑γ‑丁内酯，然后向反应体系中通入氯化氢，依次进行取代反应和水解脱羧反应，生成维生素B1中间体，即3‑氯‑5‑羟基‑2‑戊酮，催化剂包括铜盐类路易斯酸；本发明合成3‑氯‑5‑羟基‑2‑戊酮的方法能够对环境更友好、设备腐蚀性小且兼具较高收率，并且能够一锅法进行，操作更简单，生产成本更低，更适于工业化应用。

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一种藜芦醛的合成工艺

本发明涉及有机化学合成技术领域，具体为一种藜芦醛的合成工艺，具体的，以三氯氧磷、N‑甲基甲酰苯胺和邻苯二甲醚为原料，先将三氯氧磷和部分N‑甲基甲酰苯胺混合反应制成Vilsmeier试剂，再将邻苯二甲醚溶解在剩余的N‑甲基甲酰苯胺后滴加入Vilsmeier试剂中保温反应，最后将上述反应溶液水解萃取制得藜芦醛。本发明解决了现有技术中藜芦醛合成工艺中藜芦醛收率较低、制备时间较长的技术问题。

Polyetherketon, sein monomer und phenolat

一种光催化α-卤代羰基化合物的还原脱卤方法

本发明公开了一种光催化α‑卤代羰基化合物的还原脱卤方法，包括以下步骤：在LED光照条件下，将α‑卤代羰基化合物置于反应溶剂中，在室温下反应1～12小时得到反应液，将反应液分离纯化后即得到反应产物，α‑卤代羰基化合物的结构式为 反应产物的结构式为 本发明的有益之处在于：(1)、采用LED灯光催化的方法，反应条件温和，无需惰性气体保护、光催化剂、添加剂以及额外的还原剂；(2)、底物适用范围广；(3)、操作简便，反应效率高。

Organo-cascade catalysis: one-pot production of chemical libraries

A method for production of a chemical library is provided, where the method involves: reacting, in a single vessel, a) a plurality, x, of aldehydes and/or ketones; and b) either (i) a plurality, y, of nucleophiles, (ii) a plurality, z, of electrophiles or both (i) and (ii); in the presence of c) a cascade catalyst capable of catalyzing reaction between said plurality of aldehydes and/or ketones and said plurality of nucleophiles, said plurality of electrophiles or both; to obtain a mixture of x-y β-nucleophile substituted aldehydes and/or ketones, x⋅z α- electrophile substituted aldehydes and/or ketones or x⋅y⋅z β-nucleophile substituted, α- electrophile substituted aldehydes and/or ketones; and the chemical libraries thus produced.

パラジウム錯体、カップリング反応触媒、および芳香族化合物の製造方法

室温程度の温和な反応条件であっても、カップリング反応が短時間に進行し、高い収率で目的生成物が得られるパラジウム錯体を提供することであり、下記一般式（Ａ）で表される、パラジウム錯体を用いる。（式中、Ｘは、塩素原子等を表し、Ｒ１～Ｒ３は、それぞれ独立して、フッ素原子で置換されていてもよい炭素数１～６のアルキル基等を表し、Ｒ４～Ｒ６は、それぞれ独立して、炭素数１～２０のアルキル基等を表す。）

三甲基大环酮的制备方法

三甲基大环酮的制备方法，采用乙酰乙酸乙酯与1，10-二溴癸烷或1，9-二溴壬烷在均相反应条件下采用有机碱催化，生成2，15-十六烷二酮或2，14-十五烷二酮，再加入脱水硅胶进行闭环、加氢还原反应，制备3-甲基环十五酮(麝香酮)或3-甲基环十四酮。其优点是：具有可进行工业化生产等特点，是一种具有商用价值的麝香酮和3-甲基环十四酮制备方法，反应周期短、操作及后处理方便。

苯乙酮结晶废弃物资源化利用合成2,4-二氯苯乙酮的方法

本申请公开了一种苯乙酮结晶废弃物资源化利用合成2,4‑二氯苯乙酮的方法，是以2,4‑二氯苯乙酮的结晶废弃物为原料，经催化异构合成工序、负压精馏分离、发汗结晶分离获得含量99％的2,4‑二氯苯乙酮，获得的低油经多次催化异构合成后，2,4‑二氯苯乙酮的总收率可达95％以上，资源化利用苯乙酮结晶废弃物、变废为宝，节约资源、保护环境。工艺路线清洁、高效：仅通过加入适量的催化剂催化异构合成、再经精馏、结晶获得高含量产品，无废水、废气，三废处理难度小；产品收率高，低油经催化异构合成后，产品的总收率95％以上，产品纯度99％以上。

3-페닐 프로피오페논의 제조방법

본 발명은 3-페닐 프로피오페논의 제조방법에 관한 것으로, 좀더 상세하게 설명하자면, 3-클로로 프로피오닐 클로라이드를 알루미늄 클로라이드의 존재하에 벤젠과 반응시켜서 목적물질인 3-페닐 프로피오페논을 제조하는 방법이다.

一种2-烷氧基-2-环戊烯-1-酮的制备方法

本发明公开了一种制备2‑烷氧基‑2‑环戊烯‑1‑酮的方法，具体为以环戊酮和脂肪醇为反应底物，在当量碘和铜盐存在下，经由碘化、取代、氧化及加成消除的串联反应得到2‑烷氧基‑2‑环戊烯‑1‑酮。环戊酮的化学结构通式为 ，醇的化学结构通式为R 2 OH，铜盐选自乙酸铜、碘化亚铜、单质铜和氧化铜中的一种。本发明公开的制备方法具有原料易得、底物范围广、操作简单方便和绿色安全等优点。

3-甲基大环酮的制备方法

3-甲基大环酮的制备方法，属食品添加剂领域，采用乙酰乙酸乙酯与1,10-二溴癸烷或1,9-二溴壬烷在均相反应条件下采用有机碱催化，生成2,15-十六烷二酮或2,14-十五烷二酮，2,15-十六烷二酮或2,14-十五烷二酮在Ti-媒介TiCl 4 -有机胺体系，在常温常压下，加入脱水硅胶进行闭环、加氢还原反应，制备3-甲基环十五酮或3-甲基环十四酮,其优点是：具有可进行工业化生产等特点，是一种具有商用价值的麝香酮和3-甲基环十四酮制备方法，反应周期短、操作及后处理方便。

Composto, composição química aromática, uso do composto, e, método para preparar o composto

COMPOSTO, COMPOSIÇÃO QUÍMICA AROMÁTICA, USO DO COMPOSTO, E, MÉTODO PARA PREPARAR O COMPOSTO. A presente invenção se refere a 2,4-dietilacta-2,6-dienal e a um método de preparação deste, ao uso de 2,4-dietilacta-2,6-dienal como produto químico aromático; ao uso de 2,4-dietilacta-2,6-dienal para preparar uma composição química aromática ou para modificar o carácter aromático de uma composição química aromática; a uma composição química aromática contendo 2,4-dietilacta-2,6-dienal; e a um método para preparar uma composição aromatizada ou para modificar o caráter aromático de uma composição aromatizada

2,4-dietilocta-2,6-dienal y su uso como producto quimico aromatico.

La presente invención se refiere a 2,4-dietilocta-2,6-dienal y a un método para prepararlo, al uso de 2,4-dietilocta-2,6-dienal como producto químico aromático; al uso de 2,4-dietilocta-2,6-dien al para preparar una composición química aromática o para modificar el carácter aromático de una composición química aromática; a una composición química aromática que contiene 2,4-dietilocta-2,6-dienal; y a un método para preparar una composición aromatizada o para modificar el carácter aromático de una composición aromatizada.

一种光电材料中间体1-溴芴酮的合成方法

本发明公开了一种光电材料中间体1‑溴芴酮的合成方法，属于有机化学合成技术领域。该方法是以间二溴苯为原料合成2，6‑二溴苯甲酸，然后与亚硫酰氯反应合成2，6‑二溴苯甲酰氯，再与苯傅克反应合成2，6‑二溴二苯甲酮，再经分子内关环得到目标化合物1‑溴芴酮。利用本发明技术方案合成化合物1‑溴芴酮，其生产成本低、操作简单，适合工业化生产。采用本发明合成化合物1‑溴芴酮，工艺中后处理产生的危害物质及三废较少，有利于环保；并且收率高。

一种藜芦醛的合成工艺

本发明涉及有机化学合成技术领域，具体为一种藜芦醛的合成工艺，具体的，以三氯氧磷、N‑甲基甲酰苯胺和邻苯二甲醚为原料，先将三氯氧磷和部分N‑甲基甲酰苯胺混合反应制成Vilsmeier试剂，再将邻苯二甲醚溶解在剩余的N‑甲基甲酰苯胺后滴加入Vilsmeier试剂中保温反应，最后将上述反应溶液水解萃取制得藜芦醛。本发明解决了现有技术中藜芦醛合成工艺中藜芦醛收率较低、制备时间较长的技术问题。

一种5-氯-1-茚酮的制备方法

本发明涉及化学合成领域，具体涉及一种5‑氯‑1‑茚酮的制备方法。主要特点在于烷基化反应过程中加入相转移催化剂，相转移催化剂的作用是降低了烷基化反应温度，提高产品合成收率；更重要的是提高了烷基化反应体系的流动性，相对低温下进行三氯化铝水解处理过程中可实现自动化匀速滴加，操作方便，节省人力物力，有利于工业化生产。

去甲肾上腺酮盐酸盐的合成方法

本发明公开了去甲肾上腺酮盐酸盐的合成方法。该方法包括：(1)使式I所示化合物与乌洛托品进行第一反应，得到式II所示化合物；(2)将式II所示化合物与盐酸混合，并进行第二反应，得到式III所示化合物去甲肾上腺酮盐酸盐；该方法具有操作安全简便、反应速度快、原料反应完全、产物收率高等优点。

一种光电材料中间体1-溴芴酮的合成方法

本发明公开了一种光电材料中间体1‑溴芴酮的合成方法，属于有机化学合成技术领域。该方法是以间二溴苯为原料合成2，6‑二溴苯甲酸，然后与亚硫酰氯反应合成2，6‑二溴苯甲酰氯，再与苯傅克反应合成2，6‑二溴二苯甲酮，再经分子内关环得到目标化合物1‑溴芴酮。利用本发明技术方案合成化合物1‑溴芴酮，其生产成本低、操作简单，适合工业化生产。采用本发明合成化合物1‑溴芴酮，工艺中后处理产生的危害物质及三废较少，有利于环保；并且收率高。

一种2-烷基茚满-1-酮类化合物的制备方法

本发明公开了一种2‑烷基茚满‑1‑酮类化合物的制备方法，包括在导向基和铑催化剂存在下，原料化合物I‑0进行分子内烯烃“一碳”插入非张力酮碳碳键反应，反应后处理得到2‑烷基茚满‑1‑酮类化合物。本发明公开的2‑烷基茚满‑1‑酮类化合物的制备方法，选择性高，有利于提高反应的转化率，提高目标产物的收率；有利于2‑烷基取代的茚满‑1‑酮类化合物的纯化操作，有利于提高目标产品的纯度；合成路线简单，易于合成；方法简便易操作，条件温和，无安全隐患，无环境污染，有利于工业化广泛推广以及生产应用。

2,4-二乙基辛-2,6-二烯醛及其作为芳香化学品的用途

本发明涉及2,4‑二乙基辛‑2,6‑二烯醛及其制备方法，涉及2,4‑二乙基辛‑2,6‑二烯醛作为芳香化学品的用途；涉及2,4‑二乙基辛‑2,6‑二烯醛用于制备芳香化学组合物或用于改变芳香特性的用途；涉及一种包含2,4‑二乙基辛‑2,6‑二烯醛的芳香化学组合物；涉及一种制备加香组合物或改变加香组合物芳香特性的方法。

一种帕立骨化醇20s异构体杂质的制备方法

本发明属于有机化学领域，公开了一种的帕立骨化醇20S异构体杂质制备方法，包含以下步骤：步骤一：化合物1在有机溶剂一中与氧化剂反应得到化合物2；步骤二：化合物2在有机溶剂二中于碱性条件下与含硅基的羟基保护基试剂反应得到化合物3；步骤三：化合物3在有机溶剂三中于碱性条件下与化合物4进行偶联反应得到化合物5；步骤四：化合物5在有机溶剂四中与脱硅基保护基试剂反应得到化合物6(帕立骨化醇20S异构体杂质)。本发明创新点在于：首次公开了一种以全新化合物1为起始物料，并采用汇聚法定向合成帕立骨化醇20S异构体杂质；该合成方法反应条件温和、环境友好、收率高，总收率为72％，大幅降低了制备该杂质的研发成本。

一种盐酸多巴胺的制备方法

本发明涉及一种盐酸多巴胺的制备方法，该方法以3,4‑二羟基苯甲醛为起始原料，依次进行上保护反应、加成反应、还原反应得到盐酸多巴胺粗品，最后经乙醇精制得到成品。本发明所使用的原辅料均易得，反应过程中避免了使用高污染试剂，绿色环保，且整个反应路线适中、操作简便，反应条件温和，所得成品盐酸多巴胺收率高，质量好，有利于实现工业化生产。

一种偕二氟烯烃化合物的制备方法

本发明公开了一种偕二氟烯烃化合物的制备方法，将三氟甲基烯烃化合物在二苯基氧膦、碳酸铯的作用下，于溶剂中进行加氢脱氟反应，得到偕二氟烯烃化合物。本发明反应条件温和，官能团耐受性好，具有良好的区域选择性。

环丙基甲醛的合成新方法

本发明公开了一种合成环丙基甲醛的新方法，将丙烯醛为与重氮甲烷在溶剂中在Pd(oAc) 2 催化剂作用下，进行脱氮环化反应，得到环丙基甲醛粗品，再经酸洗、过滤分层、常压精馏得到含量99%以上的纯品，收率90%以上。该合成路线条件温和，副产少，收率高，环境友好，较适合于工业化放大。

一种光催化α-卤代羰基化合物的还原脱卤方法

本发明公开了一种光催化α‑卤代羰基化合物的还原脱卤方法，包括以下步骤：在LED光照条件下，将α‑卤代羰基化合物置于反应溶剂中，在室温下反应1～12小时得到反应液，将反应液分离纯化后即得到反应产物，α‑卤代羰基化合物的结构式为 反应产物的结构式为 本发明的有益之处在于：(1)、采用LED灯光催化的方法，反应条件温和，无需惰性气体保护、光催化剂、添加剂以及额外的还原剂；(2)、底物适用范围广；(3)、操作简便，反应效率高。

一种维生素b1中间体的绿色合成方法

本发明公开了一种维生素B1中间体的绿色合成方法，在催化剂存在下使α‑乙酰基‑γ‑丁内酯在有氧条件下、在溶剂中反应，生成α‑羟基乙酰基‑γ‑丁内酯，然后向反应体系中通入氯化氢，依次进行取代反应和水解脱羧反应，生成维生素B1中间体，即3‑氯‑5‑羟基‑2‑戊酮，催化剂包括铜盐类路易斯酸；本发明合成3‑氯‑5‑羟基‑2‑戊酮的方法能够对环境更友好、设备腐蚀性小且兼具较高收率，并且能够一锅法进行，操作更简单，生产成本更低，更适于工业化应用。

一种2,3,4-三羟基苯甲醛的合成方法

本发明提供一种2,3,4‑三羟基苯甲醛的合成方法，所述2,3,4‑三羟基苯甲醛的合成是以邻苯三酚为起始原料，经过保护酚羟基、甲酰化、脱保护三个步骤。本发明原料廉价易得，操作简单，产品收率和纯度高，三废量少，所述方法具有优异的经济和环保效益。

一种2-烷氧基-2-环戊烯-1-酮的制备方法

本发明公开了一种制备2‑烷氧基‑2‑环戊烯‑1‑酮的方法，具体为以环戊酮和脂肪醇为反应底物，在当量碘和铜盐存在下，经由碘化、取代、氧化及加成消除的串联反应得到2‑烷氧基‑2‑环戊烯‑1‑酮。环戊酮的化学结构通式为 ，醇的化学结构通式为R 2 OH，铜盐选自乙酸铜、碘化亚铜、单质铜和氧化铜中的一种。本发明公开的制备方法具有原料易得、底物范围广、操作简单方便和绿色安全等优点。

一种1-溴芴酮的制备方法

本发明公开了一种1‑溴芴酮制备方法，属有机化学合成领域。通过如下方法实现：以2‑溴苯乙腈为起始原料，与硝基苯反应后合成3‑(2‑溴苯基)‑5‑苯并异噁唑；3‑(2‑溴苯基)‑5‑苯并异噁唑经铁粉还原得2‑氨基苯‑2’‑溴苯甲酮，最后经分子内环化合成1‑溴芴酮，其含量99.5%(HPLC)以上，总收率76%以上。合成方法生产成本低，适合工业化生产。1‑溴芴酮可用于有机光电材料、生物医药、染料等领域。

苯乙酮结晶废弃物资源化利用合成2,4-二氯苯乙酮的方法

本申请公开了一种苯乙酮结晶废弃物资源化利用合成2,4‑二氯苯乙酮的方法，是以2,4‑二氯苯乙酮的结晶废弃物为原料，经催化异构合成工序、负压精馏分离、发汗结晶分离获得含量99％的2,4‑二氯苯乙酮，获得的低油经多次催化异构合成后，2,4‑二氯苯乙酮的总收率可达95％以上，资源化利用苯乙酮结晶废弃物、变废为宝，节约资源、保护环境。工艺路线清洁、高效：仅通过加入适量的催化剂催化异构合成、再经精馏、结晶获得高含量产品，无废水、废气，三废处理难度小；产品收率高，低油经催化异构合成后，产品的总收率95％以上，产品纯度99％以上。

一种连续化合成甲基异丙基酮的方法

本发明提供一种连续化合成甲基异丙基酮的方法，在n级依次串联的反应釜中进行连续化合成甲基异丙基酮。本发明方法，制备的甲基异丙基酮纯度达99%以上，收率73‑78%。本发明的方法能够实现甲基异丙基酮的连续化工业生产，减少人工参与的操作，降低运行成本，原料投入配比、原料投入量和反应时间都能够进行精确控制，可实现自动化控制，工业化生产过程更为安全、环保、可靠。

一种3,5-二卤三氟苯乙酮及其衍生物的制备方法

本申请涉及化工制药的技术领域，尤其是涉及一种3,5‑二卤三氟苯乙酮及其衍生物的制备方法，以3‑卤素‑4‑硝基三氟苯乙酮为原料，经过还原反应、卤代反应和氨基取代反应，最终得到3,5‑二卤三氟苯乙酮的衍生物，其原料便宜易得，工艺简单，条件温和，具有大规模生产的前景，具有较好的经济效应。

制备丝柏油醇金属化合物及复合物的方法

本发明提供一种制备丝柏油醇金属化合物或丝柏油醇铵化合物的方法，包括：将丝柏油醇溶于水溶性有机溶剂，得到丝柏油醇浓度为6~25mol/L的丝柏油醇溶液；将所得丝柏油醇溶液与水溶性金属盐或铵盐的水溶液在室温下充分混合反应，所述的水溶性金属盐选自常温下溶解度不低于35g/100ml的金属盐，或所述的水溶性金属盐或铵盐的水溶液浓度常温下不低于25%；所述的水溶性金属盐或铵盐的水溶液进一步优选所述水溶性金属盐在30~50℃下的饱和溶液；控制所述的水溶性金属盐或铵盐与所述的丝柏油醇的摩尔比在1：0.9~5，制备得到丝柏油醇金属化合物或丝柏油醇铵化合物溶液。本发明的方法可以根本性地改善丝柏油醇遇光易分解的不稳定特性，避免使用酸溶液造成的废水环境污染负荷及其处理成本。

一种提高5-氯-1-茚酮收率的合成方法

本发明提供一种提高5‑氯‑1‑茚酮收率的合成方法，属于有机合成的技术领域。制备方法为：以3,4’‑二氯苯丙酮为原料，加入非质子酸催化剂后加热至熔融状态，然后加入相转移催化剂进行反应。所述非质子酸催化剂为AlCl 3 、ZnCl 2 、InCl 3 、TiCl 4 、BF 3 、Fe(CF 3 SO 3 ) 3 、Fe(CF 3 SO 3 ) 2 、γ‑氧化铝中的一种；所述相转移催化剂为四丁基溴化铵、四丁基氯化铵、三辛基甲基氯化铵、苄基三乙基氯化铵、十二烷基三甲基氯化铵、十八冠六、十五冠五、聚乙二醇400、聚乙二醇600、聚乙二醇800中的一种。本发明通过加入相转移催化剂，明显的提高了傅克反应的选择性，降低了副反应的发生，提高了反应收率。

一种提高5-氯-1-茚酮收率的合成方法

本发明提供一种提高5‑氯‑1‑茚酮收率的合成方法，属于有机合成的技术领域。制备方法为：以3,4’‑二氯苯丙酮为原料，加入非质子酸催化剂后加热至熔融状态，然后加入相转移催化剂进行反应。所述非质子酸催化剂为AlCl 3 、ZnCl 2 、InCl 3 、TiCl 4 、BF 3 、Fe(CF 3 SO 3 ) 3 、Fe(CF 3 SO 3 ) 2 、γ‑氧化铝中的一种；所述相转移催化剂为四丁基溴化铵、四丁基氯化铵、三辛基甲基氯化铵、苄基三乙基氯化铵、十二烷基三甲基氯化铵、十八冠六、十五冠五、聚乙二醇400、聚乙二醇600、聚乙二醇800中的一种。本发明通过加入相转移催化剂，明显的提高了傅克反应的选择性，降低了副反应的发生，提高了反应收率。

一种三唑卡宾催化制备氘代醛的方法

本发明提供一种制备氘代醛的新方法，包括：以氘代甲醇为氘代试剂，在催化剂及碱存在下，发生醛的氢氘交换反应，得到氘代醛。本发明通过使用氘代甲醇作为氘代试剂，三唑卡宾盐作为催化剂前体，在碱的作用下有效地实现了醛的氘代，且醛的氘代率高达98％。并且反应的底物适用性广泛，不仅可以实现芳基醛的氘代，还可以实现烷基和烯基醛的氘代，且反应都能获得中等到良好的氘代率。这个无金属催化的氢氘交换反应，通过卡宾活化醛的方法实现反应的氢氘交换，减少反应步骤，提高了原子的经济性，并且底物的适用性广泛。使用卡宾作为催化剂，无需使用昂贵的贵金属作为催化剂，降低了反应的成本，使本反应具有很高的经济性和适用性。

一种硫酸特布他林的制备方法

本发明公开了一种硫酸特布他林的制备方法，该方法采用3,5‑二羟基苯乙酮为起始原料，先经苄基保护后得到3,5‑二苄氧基苯乙酮，3,5‑二苄氧基苯乙酮经过溴化铜溴代、DMSO氧化得到3,5‑二苄氧基苯乙酮醛，然后与叔丁胺还原胺化生成1‑[3,5‑二(苄氧基)苯基]‑2‑(叔丁基氨基)乙醇，最后经过氢化脱苄和硫酸成盐得到硫酸特布他林。与现有技术相比，本发明所使用的原辅料均价廉易得，避免使用高危剧毒试剂，没有高温高压反应，操作简便，反应条件温和，解决了现有工艺中步骤长收率低，具有安全隐患等缺点。

一种二烯醛或二烯酮类化合物的合成方法

本发明公开了一种二烯醛或二烯酮化合物的合成方法，其以烯醛或烯酮为起始原料，钯化合物为催化剂，氧气为氧化剂，三氟乙酸为添加剂，在极性有机溶剂中经一步脱氢反应合成得到（ E ， E ）‑二烯醛和（ E ， E ）‑二烯酮类化合物。本发明方法实现了过渡金属催化氧化脱氢合成单一立体构型的（ E ， E ）‑二烯醛和（ E ， E ）‑二烯酮类化合物，其与传统方法相比原料便宜易得，操作简单，底物适应范围更广，反应效率更高，环境友好，产率高，原子利用率高。

一种乙酰丙酮盐的制备工艺

本发明公开了一种乙酰丙酮盐的制备工艺，采用金属化合物与乙酰丙酮通过加压方式配合催化剂的作用，直接促使乙酰丙酮与金属化合物完全反应制得乙酰丙酮盐，通过对压力的控制使反应体系内的物料流动性增加，无需特殊处理和其他大量溶液作为分散介质，也无需强力剪切即可让物料充分混合反应，反应均匀且彻底，得到产品质量更加均匀稳定，且本发明的技术方案反应速度快、反应条件温和易于控制，过程无无废液产生，消除了对环境的污染，降低了产品的成本，并且原料的工艺损失少，有利于提高产品的收率，以乙酰丙酮计，成品乙酰丙酮盐收率在95％以上。

制备(4s)-或(4r)-3,4-二羟基-2,6,6-三甲基环己-2-烯酮的方法

本发明涉及制备3,4‑二羟基‑2,6,6‑三甲基环己‑2‑烯酮对映体之一的新方法，以及制备(3S，3'S)‑虾青素的方法，该方法包括：提供3,4‑二羟基‑2,6,6‑三甲基环己‑2‑烯酮的(4S)‑对映体的步骤。

一种负载型氧化铼催化柑青醛制备环柑青醛的方法

本发明提供了一种以Re 2 O 7 /AC为催化剂，催化柑青醛环化反应转化为环柑青醛的新方法。该方法以有机小分子试剂做反应溶剂，以Re 2 O 7 /AC为催化剂，在温和条件下将4‑(4‑甲基‑3‑戊烯基)‑3‑环己烯醛(对位柑青醛)和3‑(4‑甲基‑3‑戊烯基)‑3‑环己烯醛(间位柑青醛)选择环化制备环柑青醛(1,2,3,4,5,6,7,8‑八氢‑,8,8‑二甲基‑2‑萘醛和1,2,3,4,5,6,7,8‑八氢‑5,5‑二甲基‑2‑萘醛)。与传统环柑青醛生产方法相比，本发明具有鲜明特色：反应条件温和、目标产物选择性高、反应速度快；催化剂为活性炭负载的氧化铼，可循环使用、避免了传统催化废酸液的产生、环境友好。

连续流反应制备1-氯-1-乙酰基环丙胺的方法

本发明公开了连续流反应制备1‑氯‑1‑乙酰基环丙胺的方法，属于精细化工制备工艺技术领域。在连续流装置里，采用计量泵同时将3,5‑二氯‑2‑戊酮和氯仿混合溶液，氢氧化钠水溶液和四丁基氯化铵混合溶液同时泵入，在50‑60℃下反应结束转移至低温区域进行淬灭。本发明采用连续流反应器代替釜式反应，减少了产品与碱的接触时间，降低了焦油等副产物，提高了收率。