Способ получения ацетальдегида

Способ получения ацетона или ацетальдегида

VERFAHREN ZUR HERSTELLUNG VON 1,4-BUTANDIAL

Verfahren zur katalytischen Hydrolyse von alpha,beta-ungesättigten Carbonylverbindungen.

Verfahren zur Herstellung von 6-Alkoxycyclodekanonen-(1) bzw. deren Oximen

A process for the manufacture of benzodiazepine derivatives

Compounds of the general formula (wherein R represents an alkyl, alkenyl, hydroxyalkyl or aralkyl group, R1 represents an alkyl or aryl group, R2 represents an alkyl, alkoxy or trifluoromethyl group or a halogen atom, R3 represents a trifluoromethyl, alkyl, alkoxy, alkylthio, hydroxyalkylthio, nitro, amino, alkylsulphinyl, alkylsulphonyl, hydroxy or acylamino group or a halogen atom and R4, which can only be present if R3 is other than a trifluoromethyl group, represents any of the values of R3 except the latter value, and wherein the broken lines denote optional substituents) are prepared by reacting a benzophenone derivative of the general formula (wherein X represents a halogen atom) with ammonia, heating any uncyclized product obtained to effect ring closure and, in the case where R3 and R4 were absent in the benzophenone derivative, subjecting the benzodiazepine formed to one or more of the steps nitration, reduction of the nitro group and acylation ...

Novel trifluoromethyl-benzophenones and the preparation thereof

The invention comprises 2-amino-5-trifluoromethylbenzophenone and 2-amino-21, 5-bis- (trifluoromethyl)-benzophenone, and their preparation by treating the corresponding 2-chlorobenzophenones under pressure with aqueous ammonia in the presence of cuprous chloride. The biscompound is purified via its sulphate. Specification 972,976 also is referred to.

PHLOROGLUCINOL DERIVATIVES

... 1325192 Phloroglucinol derivatives ORSYMONDE 6 May 1971 [6 May 1970] 21865/70 Heading C2C Novel compounds of Formula I in which each of R 1 , R 2 and R 3 , which may be the same or different, represents a hydrogen atom or an alkyl group; each of R 4 and R 5 , which may be the same or different, represents a hydrogen atom or an alkyl group, or R 4 and R 5 together form, with the nitrogen atom to which they are bonded, a substituted or unsubstituted heterocyclic group with 5, 6 or 7 ring atoms, optionally containing, in addition to the indicated nitrogen, a further heteroatom which is sulphur, oxygen or an additional nitrogen atom, and n is 1, 2, 3 or 4 with the proviso that, when n is 1, the group -NR 4 R 5 does not represent an unsubstituted piperidine group or a 4-(C 1-4 alkyl) piperidine group or a group of formula wherein Z is a group of either of the formulµ where R 6 is in the 2 or 4 position and represents a hydrogen atom, a chlorine atom or an alkoxy group of 1-5 carbon atoms, R ...

A-HALOMETHYLAMINO COMPOUNDS AND THEIR PREPARATION

PROCESS FOR THE PREPARATION OF BENZOYL PEROXIDE

... 1,222,269. Benzoyl peroxide. CHAS. PFIZER & CO. Inc. 4 Dec., 1968, No. 57686/68. Heading C2C. Benzoyl peroxide may be obtained by contacting benzoic anhydride or a mixture of benzaldehyde and benzoic anhydride containing 0À1 to 1 equivalent of benzoic anhydride per equivalent of benzaldehyde with oxygen in the presence of an inert reaction medium containing a catalytic amount of an alkali or alkaline earth metal sulphate or benzoate at between 0‹ and 50‹ C. The reaction mixture may be irradiated with low intensity irradiation of wavelength 180 mÁ to 400 mÁ. The mixture of benzaldehyde and benzoic anhydride may be prepared by contacting benzalchloride and also, if desired, benzotrichloride with 0À1 to 1 equivalent of benzoic acid per equivalent of benzalchloride or the chloride mixture, and when benzotrichloride is present the amount of benzoic acid is sufficient to provide at least 1 equivalent per equivalent of benzalchloride, in the presence of at least 0À1% by weight of an electrophilic ...

BUTANONE DERIVATIVES PROCESS FOR PREPARATION THEREOF AND THE ORGANOLEPTIC USE THEREOF

PROCESS AND INTERMEDIATES FOR THE PREPARATION OF 2-SUBSTITUTED BENZALDEHYDES

Process for the preparation of derived from 1,4-benzodiapine.

Process for the preparation of derived from 1,4-benzodiazepine.

Process for the preparation of derived from 1,4-benzodiazepine.

Process for the preparation of derived from 1,4-benzodiazepine.

Process for the preparation of derived from benzodiazepine.

Process for the preparation of derived from 1,4-benzodiazepine.

Preparation of méta-aryloxy-benzaldéhydes.

Process for the preparation of derived from 1,4-benzodiazepine.

Process for the preparation of derived from 1,4-benzodiazepine.

PROCESS AND INTERMEDIATES FOR THE PREPARATION OF 2-SUBSTITUTED BENZALDEHYDES

PROTECTED ONE 3,5-DIHYDROXY-2,2-DIMETHYL VALERONITRILE FOR the SYNTHESIS OF EPOTHILONEN AND DERIVATIVES AND PROCEDURE FOR the PRODUCTION AND the USE

PROCEDURE FOR THE PRODUCTION OF MAKROCYCLI KETONE

VERFAHREN ZUR HERSTELLUNG VON GLYOXAL, ALKYLGLYOXALEN UND VON DEREN ACETALEN

STEUERSCHALTUNG ZUM STOPPEN ODER ANHALTEN BUERSTENLOSER GLEICHSTROMMOTOREN

GATE CIRCUIT FOR STOPPING OR STOPPING BRUSHLESS DIRECT CURRENT MOTORS

PROCEDURE FOR THE PRODUCTION OF SQUARIC ACID

PROCEDURE FOR THE PRODUCTION OF M-HALOGENMETHYL DIPHENYLAETHERN

PROCEDURE FOR THE PRODUCTION OF HYDROXYLIERTER ISOFLAVONEN

PROCEDURE FOR the PRODUCTION OF 4-ARYLDISUBSTITUIERTEN-1-TETRALONEN.

HYDROLYSIS OF ACTIVATED OLEFINI ALDEHYDES AND KETONEN.

3-HYDROXY-2-CYCLOBUTEN-1-ON-SALZE, THEIR PRODUCTION AND USE.

INTERMEDIATE CONNECTIONS TO THE SYNTHESIS OF CARBONIC ACIDS.

PROCEDURE FOR the PRODUCTION OF 2-ALKYL-1,4BUTANDIAL.

PROCEDURE FOR THE PRODUCTION OF TEREPHTHALALDEHYD AND/OR ISOPHTHALALDEHYD.

Carbonylated compounds preparation process from a vegetable product and resulting carbonylated compounds

Process for preparing hydrofluoroethers

Beta-aminovinyl ketones, preparation method therefor and use thereof for preparing beta diketones

Method for preparing hydrazine hydrate

IMPROVED PROCESS FOR PREPARING HYDRAZINE HYDRATE WITH PYRAZOLINE RECYCLING

La présente invention concerne un procédé amélioré de préparation d'hydrate d'hydrazine à partir de l'azine de la méthyl éthyl cétone obtenue à partir de la méthyl éthyl cétone par oxydation de l'ammoniac par l'eau oxygénée en présence d'un activateur, caractérisé en ce qu'il comprend une étape de recyclage de la purge des hétérocycles de la famille de la pyrazoline.

PROCESS FOR PREPARING 4-HYDROXY, 2,4,6-TRIMETHYL CYCLOHEXA-2,5-DIENONE

L'invention concerne un procédé de préparation de l'hydroxy-4 triméthyl-2,4,6 cyclohexadiène-2,5 one par chloration du triméthyl-2,4,6 phénol par le chlore dans un solvant organique en l'absence de base en éliminant l'acide chlorhydrique gazeux forme au fur et à mesure de sa formation, par toute méthode physique appropriée suivie de l'hydrolyse du mélange réactionnel par l'eau éventuellement en présence d'une base minérale.

PROCESS FOR THE PREPARATION OF 1-ARYLOXY-METHYL KETONES

A process for the preparation of a 1-aryloxy-methyl ketone of the formula in which R1, R2 and R3 each independently is hydrogen, optionally substituted alkyl, alkenyl, alkynyl or optionally substituted aryl, or R1 and R2 together are an alkylene chain, R4 each independently is halogen, alkyl, alkoxy, optionally substituted aryl or nitro, and n is 0, 1, 2 or 3, comprising hydrolyzing a 1-halogeno-2-aryloxy-1-alkene of the formula in which Hal is chlorine or bromine, under acidic conditions at a temperature from about 20 to 150.degree.C,until it is about 95 to 100% complete, adding a base, and then bringing the reaction to completion under weakly alkaline conditions at about 20 tO 150.degree.C. Advantageously all stages of the reaction are effected in a single vessel at a temperature from about 40 to 100.degree.C and in the presence of an inert organic solvent, optionally in admixture with water as a solution or as a two-phase system, about 1 mol of a monobasic acid and 2 mols ...

METHOD FOR THE PREPARATION OF CARBONYL PRODUCTS STARTING FROM HYDROCARBON AMS COMING FROM STEAM-CRACKING INSTALLATIONS

INDENYL ACETIC ACIDS AND PROCESSES FOR PREPARING SAME

PROTECTED 3.5-DIHYDROXY-2,2-DIMETHYL-VALERONITRILES FOR THE SYNTHESIS OF EPOTHILONES AND EPOTHILONE DERIVATIVES AND PROCESS FOR THE PRODUCTION AND THE USE

The invention relates to 3.5-dihydroxy-2.2-dimethyl-valeronitriles for the synthesis of epothilone and epothilone derivatives and a method for producing said novel intermediate products in the synthesis and the use thereof in the production of epothilones or epothilone derivatives.

CARBOCATALYSTS FOR CHEMICAL TRANSFORMATIONS

The disclosure relates to catalytically active carbocatalysts, e.g., a graphene oxide or graphite oxide catalyst suitable for use in a variety of chemical transformations. In one embodiment, it relates to a method of catalyzing a chemical reaction of an organic molecule by reacting the organic molecule in the presence of a sufficient amount of graphene oxide or graphite oxide for a time and at a temperature sufficient to allow catalysis of a chemical reaction. According to other embodiments, the reaction may be an oxidation reaction, a hydration reaction, a dehydrogenation reaction, a condensation reaction, or a polymerization reaction. Some reactions may include auto-tandem reactions. The disclosure further provides reaction mixtures containing an organic molecule and graphene oxide or graphite oxide in an amount sufficient to catalyze a reaction of the organic molecule.

15,16-SECO-19-NOR PROGESTINS

... 2071917 9204309 PCTABS00011 15,16-Seco-19-nor progestins are provided which display elevated progestational activity with a minimum of ancillary hormonal activity. Processes for the preparation of the novel progestins are provided as are methods of use. A preferred method of use is in the suppression of ovulation in the human female.

CHLORINATION OF SUBSTITUTED ALKENES USING TRICHOLORISOCYANURIC ACID

This invention relates to a process for the selective monochlorination or dichlorination of certain substituted alkenes using trichloroisocyanuric acid. T he chlorinated alkenes can be easily hydrolyzed to provide .alpha.-monochloroketone s or .alpha.,.alpha.-dichloroketones with a high degree of selectivity. The resulting .alpha.-monochloroketones or .alpha.,.alpha.-dichloroketones have utility as fun gicides or function as useful intermediates for fungicides.

SYNTHESES OF D-CHIRO-3-INOSOSE AND (+)-D-CHIRO-INOSITOL

There are described novel biocatalytic and chemical processes for the synthesis of various oxygenated compounds. Particularly, there are described processes for the synthesis of a useful synthon (12) made by reacting a protected diol (acetonide) with permanganate under appropriate conditions. Such synthon is useful of the synthesis of various pharmaceutically important compounds such as D-chiro-inositol and D-chiro-3-inosose. Also, there are disclosed novel compounds, including specifically the synthon (12) and compounds derived therefrom.

Verfahren zur Darstellung von Oxymethylenphenylacetaldehyd.

Verfahren zur Darstellung von 2,4,6,2'-Tetraoxybenzophenon (Salicylophloroglucin)

Procédé de préparation d'un nouveau dérivé de la tétrahydronaphtaline.

Verfahren zur Herstellung von Moschusriechstoffen

Verfahren zur Darstellung von Phlorisocapronophenon.

Verfahren zur Darstellung von Resisocapronophenon.

Verfahren zur Herstellung von fluorhaltigen Benzodiazepinen

Verfahren zur Herstellung von Cyclododecanon

Procédé de préparation de 2-octalones

Phloroglucinol amino ketones

Phloroglucinol amino ketones. Cpds. (I), useful as antispasmodics and vasodilators: (where R1, R2 and R3 are H or alkyl (esp. 1-5C alkyl); R4 and R5 are H or alkyl (esp. 1-5C alkyl) or NR4R5 is a 5-7 membered heterocyclic ring opt. contg. an additional O, S or N atom and opt. substd. by alkyl, aryl, amino, alkylamino, hydroxyl, hydroxyalkyl, anilido or N-alkylacetamido and n is 1-4) are prepd. by reacting a 1,3,5-trihydroxybenzene deriv. with either NC(CH2)nNR4R5 and hydrolysing the ketimine formed or NC(CH2)nCl and reacting the - -chloroalkanophenone with R4R5NH.

Alicyclic ketones - useful aromatising agents

Cpds. I (A,B) where either (A) m and n = 0 or 1, the ring contains a double bond at position 1,2(exocyclic), 3 or 4, or two conjugated double bonds on positions 1 and 3, the side chain on the 1-position of the ring may contain a double bond on the 2' or 3' position as shown by the dotted lines, R1 and R2 are both H or one a 1-6C alkyl and the other H; R3, R4 and R5=H or one may=1-6C alkyl and the others=H, and X=O (if m=0 and n=1) or OH (if m=n=0); or (B) where m=n=1, the ring contains a double bond at position 1,2(endocyclic), 3 or 4, or two conjugated double bonds at positions 1 and 3, the side chain on the 1-position of the ring may contain a double bond in the 2' position as indicated by the dotted line, R1-5 have the same meaning as above and X=OH. The cpds. are useful as aromatising agents in perfumes, foodstuffs, animal feeds, drinks, pharmaceutical agents and tobacco products.

Alicyclic ketones - useful aromatising agents

Cpds. I (A,B) where either (A) m and n = 0 or 1, the ring contains a double bond at position 1,2(exocyclic), 3 or 4, or two conjugated double bonds on positions 1 and 3, the side chain on the 1-position of the ring may contain a double bond on the 2' or 3' position as shown by the dotted lines, R1 and R2 are both H or one a 1-6C alkyl and the other H; R3, R4 and R5=H or one may=1-6C alkyl and the others=H, and X=O (if m=0 and n=1) or OH (if m=n=0); or (B) where m=n=1, the ring contains a double bond at position 1,2(endocyclic), 3 or 4, or two conjugated double bonds at positions 1 and 3, the side chain on the 1-position of the ring may contain a double bond in the 2' position as indicated by the dotted line, R1-5 have the same meaning as above and X=OH. The cpds. are useful as aromatising agents in perfumes, foodstuffs, animal feeds, drinks, pharmaceutical agents and tobacco products.

Verfahren zur Herstellung von 1,4-Benzodiazepinen

Verfahren zur Herstellung von Benzophenonderivaten

Verfahren zur Herstellung von 1,4-Benzodiazepin-Derivaten

Verfahren zur Herstellung von 1,4-Benzodiazepin-Derivaten

Verfahren zur Herstellung von 1,4-Benzodiazepin-Derivaten

Verfahren zur Herstellung von 1,4-Benzodiazepinen

Verfahren zur Herstellung von 1,4-Benzodiazepinen

Verfahren zur Herstellung von 1,4-Benzodiazepin-Derivaten

Verfahren zur Herstellung von 1,4-Benzodiazepinen

Verfahren zur Herstellung von 2,6-Dichlorbenzalchlorid

Verfahren zur Herstellung von 3,5-Diniederalkoxy-homophthalsäuren

Verfahren zur Herstellung von Benzodiazepin-Derivaten

Verfahren zur Herstellung neuer Oxime

Procédé de préparation d'un composé aminocétonique du phloroglucinol

[...] DE [...] D' [...][...][...].

Process for the preparation of carbonyl products from hydrocarbon streams coming from steam cracker plants

The technical problem of recovering acetylenic compounds from steam-cracking streams without hydrogenation of such compounds is solved by adding an alcohol to these streams in the presence of an ion exchange resin in which the acidic centres have been exchanged with Hg<++> ions and alkali metal ions and alkaline earth metal ions, carrying out a rectification in order to recover the product thus formed, hydrolysing the latter by means of an acidic ion exchange resin and separating the carbonyl compound thus obtained by means of rectification operations.

Process for the alkylation of carbonyl compounds and products thus obtained

The monoalkylation/aldo condensation or the monoalkylation/aldo condensation/dehydration of a carbonyl compound is obtained with good yields by reacting an imine of the carbonyl compound with an alpha , beta -ethylenic carbonyl compound in an equimolar ratio or in a molar ratio equal to 0.25 respectively, followed by hydrolysis and neutralisation of the compound obtained. These reactions are carried out without ending in self-condensation products or in polyalkylations.

Aryl-alkane acids production - forming an aldehyde from aryl or alkyl groupings and converting

An acids of formula ARCH(CH3)COOH(I) (where Ar is aryl) are prepd. by (a) dehydrating and then hydrolysing a cpd. of formula AR2C(CH3)(OH)CH2NR1R2 (II) (where R1 and R2 are each alkyl or aryl or together with the nitrogen form a 5-7 ring) to create an aldehyde of formula Ar1CH(CH3)CHO (III) and, (b) converting the aldehyde of formula (III) to an acid of formula (i) (where Ar1 is Ar or a group convertible during (b) to Ar, and AR2 is Ar1 or a group convertible during (a) to Ar1).

PROCEDURE FOR THE PRODUCTION OF SQUARIC ACID.

PROCEDURE FOR THE PRODUCTION OF M-ARYLOXYBENZALDEHYDEN.

Process for the preparation of benzene derivatives

... p-tert-Butylbenzene derivatives are obtained by a novel process by reacting p-tert-butyltoluene with chlorine at temperatures of about 5-35 DEG C, under the action of energy-rich radiation and/or in the presence of free radical initiators, and, if desired, the p-tert-butylbenzyl chloride obtained, optionally after purification, is converted into p-tert-butylbenzaldehyde by methods known per se. The products obtained by the novel process are known substances, in particular of intermediate character.

COMPOUNDS WITH THERAPEUTIC ACTIVITY, IN PARTICULAR AS ANTI-PHENALEN, COMPOSITIONS CONTAINING THEM AND METHODS FOR THEIR PREPARATION.

ALPHA HALOGEN METHYL AMINO ACIDS.

Process for the preparation of 3-phenoxybenzaldehyde

Prodn. of antiinflammatory 4-naphthyl-2-butanone deriv.

Prodn. of 4-(6-methoxy-2-naphthyl)- 2-butanone of formula (I) is effected by (a) reacting a 6-methoxy-2-naphthylmethyl halide of formula (II) with an alkali metal acetone hydrazone of formula (III), and (b) subjecting the prod. of formula (IV) to acid hydrolysis: In the formula, X=halogen; M=alkali metal; R1 and R2=1-6C alkyl.

METHOD OF SYNTHESIS OF 3.4 - DIMETHOXYBICYCLO [4.2 .0] OCTA - 1.3, 5 - TRIENE - 7 - CARBONITRILE AND APPLICATION TO THE SYNTHESIS OF IVABRADINE AND ITS ADDITION SALTS WITH PHARMACEUTICALLY ACCEPTABLE ACID

СПОСОБ ПОЛУЧЕНИЯ БИЦИКЛИЧЕСКИХ 1,3-ДИКЕТОНОВ

Изобретение относится к способу получение бициклических 1,3-дикетонов формулы I где R1, R2, R3 и R4 означают водород, C1-C4алкил, C1-C4алкоксикарбонил, галоген, пиано, нитро, C1-C4алкилтио, C1-C4алкилсульфенил и C1-C4алкилсульфонил и Z означает C1-C4алкилен, O, S, N-R5, где R5 означает C1-C4алкил и C1-C4алкилкарбонил, причем а) бициклический олефин формулы II подвергают взаимодействию с галоформом в присутствии основания с получением продукта с расширенным циклом формулы III где R1-R4 и Z имеют вышеприведенное значение и X означает галоген; и осуществляют б) гидролиз аллильного галогена соединения формулы III с получением аллильного спирта формулы IV в) окисление алилльного спирта формулы IV с получением ненасыщенного кетона формулы V г) взамодействие кетона формулы V с нуклеофильным, стабилизирующим отрицательный заряд ионом Y- с получением кетона формулы VI д) гидролиз кетона формулы VI с получением бициклического 1,3-дикетона формулы I. Отчет о международном поиске был опубликован 2002.05.02 ...

CARBON CATALYSTS FOR CHEMICAL TRANSFORMATIONS

Terminal Conjugated Trienal Acetal Compound and Method for Producing Terminal Conjugated Trienal Compound Using the Same

Preparation method of 4,4'-difluorobenzophenone

SYNTHETIC NAVEL ORANGEWORM PHEROMONE COMPOSITION AND METHODS RELATING TO PRODUCTION OF SAME

One or more embodiments of the invention are directed to the synthetic methods for making lepidopteran pheromones including navel orangeworm pheromones. The synthetic methods involve novel, efficient, and environmentally benign steps and procedures. 1{'sup': 1', '1, 'producing a compound of formula Y′—R—X (2) from a compound of formula Y—R—X (1);'}producing a compound of formula. A method for synthesizing a sex attractant pheromone of formula R—R—R—Y′ (7) comprising:{'sup': 3', '7', '1, 'producing a final compound of formula R—R—R—Y′ (7) from a compound of formula'}from said compound of formula (2); and X is halogen,', 'Y is —OH,', 'Y′ is ═O,', {'sup': '1', 'sub': 2', 'm, 'Ris [—CH—], or alkyl,'}, {'sup': '3', 'sub': 3', '2', 'n, 'Ris CH—[CH]—, or alkyl,'}, {'sup': '5', 'sub': 'p', 'Ris [—C≡C—], or alkynyl,'}, {'sup': '6', 'sub': 'q', 'Ris [—C≡C—], or alkynyl,'}, {'sup': 7', '8, 'Ris —C═C—C═C—, alkenyl, or R,'}, {'sup': '3', 'sub': 2', '3, 'W is —O-alkyl, —O—R, or —O—CH—CH,'}, {'sup': '8', 'Ris the geometric cis configuration represented by structure'}], 'wherein [{'sup': '9', 'sub': '3', 'Ris —CH, or alkyl,'}, {'sup': '10', 'sub': '(−)', 'Ris ≡C, carbon anion, or de-protonated carbon,'}, {'sup': '10', 'M is a metal, sodium, lithium, potassium, or magnesium, wherein M and Rtogether may form a salt,'}, 'm is independently 5, 6, 7, 8, 9, 10, 11 or 12,', 'n is independently 1, 2 or 3,', 'p is independently 1 or 2, and', 'q is independently 1 or 2.} This application is a continuation of U.S. patent application Ser. No. 13/372,288, filed Jun. 7, 2012, which is a continuation of U.S. patent application Ser. No. 12/763,589, now U.S. Pat. No. 8,115,035, filed Apr. 20, 2011, which is a continuation of U.S. patent application Ser. No. 12/255,951, now U.S. Pat. No. 7,737,306, filed Oct. 22, 2008, the contents of which are hereby incorporated by reference in their entirety.1. Field of the InventionOne or more embodiments of the invention relate to compositions and method for ...

CONTINUOUS PROCESS FOR CONVERSION OF LIGNIN TO USEFUL COMPOUNDS

This specification discloses an operational continuous process to convert lignin as found in ligno-cellulosic biomass before or after converting at least some of the carbohydrates. The continuous process has been demonstrated to create a slurry comprised of lignin, raise the slurry comprised of lignin to ultra-high pressure, deoxygenate the lignin in a lignin conversion reactor over a catalyst which is not a fixed bed without producing char. The conversion products of the carbohydrates or lignin can be further processed into polyester intermediates for use in polyester preforms and bottles. 1. A process for preparing a slurry comprised of lignin comprising the steps of:a. charging a composition comprised of lignin and at least one slurry liquid at 25° C. to a vessel capable of being subjected to vacuum,b. subjecting the vessel to vacuum for a time sufficient to disperse particles of the composition comprised of lignin to greater than 50% of the theoretical dispersion of the composition comprised of lignin.2. The process according to claim 1 , wherein the slurry liquid comprises water.3. The process according to claim 1 , wherein the slurry liquid comprises a hydrogen donor.4. The process according to claim 1 , wherein the vacuum is defined as a pressure less than atmospheric pressure.5. The process according to claim 4 , wherein the pressure less than atmospheric pressure is in the range of between 0.2 bar and 0.8 bar.6. The process according to claim 1 , wherein the time is sufficient to disperse the particles of lignin to greater than 75% of the theoretical dispersion.7. The process according to claim 1 , wherein the time is sufficient to disperse the particles of lignin to greater than 90% of the theoretical dispersion.8. The process according to claim 1 , wherein the process further comprises the application of mechanical agitation in which the composition comprised of lignin is mechanically mixed with the slurry liquid.9. The process according to claim 8 , ...

CONTINUOUS PROCESS FOR CONVERSION OF LIGNIN TO USEFUL COMPOUNDS

This specification discloses an operational continuous process to convert lignin as found in ligno-cellulosic biomass before or after converting at least some of the carbohydrates. The continuous process has been demonstrated to create a slurry comprised of lignin, raise the slurry comprised of lignin to ultra-high pressure, deoxygenate the lignin in a lignin conversion reactor over a catalyst which is not a fixed bed without producing char. The conversion products of the carbohydrates or lignin can be further processed into polyester intermediates for use in polyester preforms and bottles. 1. A continuous process for the conversion of lignin feedstock comprised of lignin and glucans , said process comprising:A. Slurry creation of a slurry comprised of lignin from the lignin feedstock,B. Charging the slurry comprised of lignin into a lignin conversion reactor having a lignin conversion pressure, wherein the pressure of the slurry comprised of lignin is higher than the lignin conversion pressure,C. Converting the lignin of the slurry comprised of lignin into lignin conversion products by contacting the lignin with hydrogen in the presence of a first catalyst at a lignin conversion temperature, andD. Removing the lignin conversion products from the lignin conversion reactor.2. The process of claim 1 , wherein the slurry creation comprises the steps of:a. charging the lignin feedstock comprised of lignin and at least one slurry liquid at 25° C. to a vessel capable of being subjected to vacuum,b. subjecting the vessel to vacuum for a time sufficient to disperse particles of the lignin to greater than 50% of the theoretical dispersion.3. The process of claim 1 , wherein the slurry creation comprises the steps of:a. imparting high shear forces to the lignin feedstock,b. adding a slurry liquid to the lignin feedstock after application of the high shear forces.4. The process of claim 1 , wherein the charging of the slurry comprised of lignin into the lignin conversion ...

CONTINUOUS PROCESS FOR CONVERSION OF LIGNIN TO USEFUL COMPOUNDS

This specification discloses an operational continuous process to convert lignin as found in ligno-cellulosic biomass before or after converting at least some of the carbohydrates. The continuous process has been demonstrated to create a slurry comprised of lignin, raise the slurry comprised of lignin to ultra-high pressure, deoxygenate the lignin in a lignin conversion reactor over a catalyst which is not a fixed bed without producing char. The conversion products of the carbohydrates or lignin can be further processed into polyester intermediates for use in polyester preforms and bottles. 1. An integrated process for the conversion of a ligno-cellulosic biomass feedstock comprised of lignin and carbohydrates , said process comprising:A. Pretreating the ligno-cellulosic biomass feedstock with treatment water which includes steam explosion to create a pre-treated ligno-cellulosic biomass feedstock,B. Converting at least a portion of the carbohydrates of the pre-treated ligno-cellulosic biomass feedstock into carbohydrate conversion products selected from the group consisting of alcohols, polyols, glucans, gluco-lignins and cellulose,C. Charging the lignin from the ligno-cellulosic biomass feedstock into a lignin conversion reactor having a lignin conversion pressure via a stream comprised of lignin from the ligno-cellulosic biomass feedstock,D. Converting at least a portion of the lignin of the pre-treated ligno-cellulosic biomass feedstock into lignin conversion products by contacting the lignin with hydrogen in the presence of a first catalyst at a lignin conversion temperature,E. Removing the lignin conversion products from the lignin conversion reactor.2. The process according to claim 1 , wherein converting at least a portion of the carbohydrates of the pretreated ligno-cellulosic biomass feedstock to at least one polyol produces a hydrogen donor which is used as a source of hydrogen for converting at least a portion of the lignin of the pre-treated ligno- ...

METHOD FOR PRODUCING ISOPHORONE

The invention relates to a method for producing isophorone by catalyzed aldol condensation of acetone as an educt, reprocessing the reaction product, hydrolyzing the product stream, and separating into an organic and an aqueous fraction, obtaining isophorone from the organic fraction, distillatively reprocessing the aqueous fraction, and feeding the vapors from the head of the distillative reprocessing apparatus into the hydrolysis apparatus. 1. A process for preparing isophorone , the process comprising:(i) reacting acetone via a catalysed aldol condensation in a reactor, thereby obtaining a reaction product,(ii) working-up the reaction product, thereby obtaining a stream of value,(iii) hydrolyzing the stream of value in a hydrolysis apparatus,(iv) separating the stream of value into an organic fraction and an aqueous fraction,(v) obtaining isophorone from the organic fraction,(vi) distilling the aqueous fraction in a distillative workup apparatus comprising a top and a bottom, and(vii) passing vapours from the top of the distillative workup apparatus onward into the hydrolysis apparatus.2. The process according to claim 1 , wherein water from the bottom of the distillative workup apparatus is subjected to a flash evaporation claim 1 , thereby obtaining a purified water which is recycled into the reactor.3. The process according to claim 1 , wherein the catalysed aldol condensation is performed in a liquid phase at a temperature of from 100 to 250° C. claim 1 , and a pressure of from 5 to 50 bar.4. The process according to claim 1 , wherein the catalysed aldol condensation is performed in a gas phase at a temperature of from 100 to 400° C.5. The process according to claim 1 , wherein the catalysed aldol condensation is performed in a supercritical range at a temperature of from 250 to 350° C. and a pressure of from 50 to 200 bar.6. The process according to claim 1 , wherein a homogeneous or a heterogeneous catalyst is used in the catalysed aldol condensation.7. The ...

INTERMEDIATE OF LYCOPENE AND PREPARATION METHOD OF INTERMEDIATE

The present invention relates to 2,6,10-trimethyl-3,5,9-undecatrienyl-1-aldehyde represented by formula (3), and a method for preparing this intermediate. The process route of the present invention is simple, the starting materials are available easily, and the cost is low. 2. The method according to claim 1 , characterized in that claim 1 , the 4-methyl-5 claim 1 ,5-dialkoxy-1-pentenyl-1-phosphoric acid dialkyl ester in Step I is 4-methyl-5 claim 1 ,5-dimethoxy-1-pentenyl-1-phosphoric acid dimethyl ester claim 1 , 4-methyl-5 claim 1 ,5-dimethoxy-1-pentenyl-1-phosphoric acid diethyl ester claim 1 , or 4-methyl-5 claim 1 ,5-dimethoxy-1-pentenyl-1-phosphoric acid diisopropyl ester.3. The method according to claim 1 , characterized in that claim 1 , the tetra-alkyl methylene diphosphonate in Step I is tetra-methyl methylene diphosphonate claim 1 , tetra-ethyl methylene diphosphonate claim 1 , or tetra-isopropyl methylene diphosphonate.4. The method according to claim 1 , characterized in that claim 1 , the bases in Step I is alkali metal hydrides claim 1 , alkali metal salts of alcohols or alkyl lithium; wherein the alkali metal hydride is sodium hydride or potassium hydride; the alkali metal salt of alcohols is sodium ethoxide claim 1 , sodium tert-butoxide claim 1 , or potassium tert-butoxidel; the alkyl lithium is butyl lithium.5. The method according to claim 1 , characterized in that claim 1 , in Step I the ether solvent is ether claim 1 , tetrahydrofuran or ethylene glycol dimethyl ether; the dipole aprotic solvent is dimethyl formamide claim 1 , dimethyl sulfoxide claim 1 , or hexamethyl-phosphoric triamide.6. The method according to claim 1 , characterized in that claim 1 , in Step I a molar ratio of dosage of the 3-methyl-4 claim 1 ,4-dialkoxy-1-aldehyde of formula (11) to the bases is 1: 1.0˜1.2; a molar ratio of dosage of the 3-methyl-4 claim 1 ,4-dialkoxy-1-aldehyde of formula (11) to the tetra-alkyl methylene diphosphonate is 1: 1.0˜1.3.7. The method ...

Process for preparing 4-penten-2-ynal

A process for preparing 4-penten-2-ynal of the following formula (2): CH 2 ═CHC≡CCHO  (2) the process comprising a step of hydrolyzing a 5,5-dialkoxy-1-penten-3-yne compound of the following general formula (1): CH 2 ═CHC≡CCH(OR 1 )(OR 2 )  (1) wherein R 1 and R 2 represent, independently of each other, a monovalent hydrocarbon group having 1 to 15 carbon atoms, preferably 1 to 8, more preferably 1 to 4, or R 1 and R 2 may be bonded to each other to form a divalent hydrocarbon group, R 1 -R 2 , having from 2 to 10 carbon atoms, to obtain 4-penten-2-ynal (2).

METHOD OF PRODUCING 2'-TRIFLUOROMETHYL GROUP-SUBSTITUTED AROMATIC KETONE

A method produces a 2′-trifluoromethyl-substituted aromatic ketone and includes reacting a 2-halogen-substituted benzotrifluoride compound with magnesium metal to convert the compound to a Grignard reagent; and reacting the Grignard reagent with an acid anhydride; and then hydrolyzing the resultant to produce a 2′-trifluoromethyl-substituted aromatic ketone. The method of producing a 2′-trifluoromethyl-substituted aromatic ketone enables 2′-trifluoromethyl-substituted aromatic ketone to be produced without using expensive raw materials by generating a Grignard reagent as an intermediate and reacting this Grignard reagent with an acid anhydride in an efficient productivity. The 2′-trifluoromethyl-substituted aromatic ketone that is produced by the method of producing a 2′-trifluoromethyl-substituted aromatic ketone can be used as fine chemicals, raw materials for pharmaceuticals and agrochemicals, raw materials for resins and plastics, electronics and information related materials, optical materials, and the like. 15.-. (canceled)7. The method according to claim 6 , wherein said acid anhydride is acetic anhydride claim 6 , propionic anhydride claim 6 , or butyric anhydride.8. The method according to claim 6 , wherein said 2′-trifluoromethyl-substituted aromatic ketone is 2′-trifluoromethyl acetophenone claim 6 , 2′-trifluoromethyl propiophenone claim 6 , or 2′-trifluoromethyl butyrophenone.10. The method according to claim 9 , wherein the amount of said lithium chloride is 0.01 to 3 times by mole that of said 2-halogen-substituted benzotrifluoride compound.11. The method according to claim 7 , wherein said 2′-trifluoromethyl-substituted aromatic ketone is 2′-trifluoromethyl acetophenone claim 7 , 2′-trifluoromethyl propiophenone claim 7 , or T-trifluoromethyl butyrophenone.14. The method according to claim 12 , wherein the amount of said lithium chloride is 0.01 to 3 times by mole that of said 2-halogen-substituted benzotrifluoride compound.15. The method according ...

METHOD FOR PRODUCING A CONJUGATED Z-ALKEN-YN-YL ACETATE

Provided is a method for industrially producing a conjugated Z-alken-yn-yl acetate such as Z-13-hexadecen-11-yn-yl acetate which is a sex pheromone component of a pine processionary moth, and an intermediate for the conjugated Z-alken-yn-yl acetate under mild conditions at a high yield. More specifically, provided is a method for producing a conjugated Z-alken-yn-yl acetate (5) comprising the steps of: reacting an ω-halo-2-alkynal (1) with an alkylidene triphenylphosphorane (3) through a Wittig reaction to obtain a conjugated Z-alken-yn-yl halide (4), and acetoxylating the conjugated Z-alken-yn-yl halide (4) into a conjugated Z-alken-yn-yl acetate (5). 2. The method for producing a conjugated Z-alken-yn-yl acetate according to claim 1 , wherein the conjugated Z-alken-yn-yl acetate is Z-13-hexadecen-11-yn-yl acetate. This application is a divisional of U.S. application Ser. No. 14/248,525, filed Apr. 9, 2014, which claims priority from Japanese Patent Application No. 2013-083861, filed Apr. 12, 2013, the disclosure of which is incorporated by reference herein in its entirety.The present invention relates to methods for producing a conjugated Z-alken-yn-yl acetate and an ω-halo-2-alkynal which is an intermediate thereof, particularly to a method for producing Z-13-hexadecen-11-yn-yl acetate which is a sex pheromone component of a pine processionary moth (scientific name: ), which is a forest pest insect in Europe.A pine processionary moth (scientific name: ) is an insect widely inhabiting European countries such as France, Italy, Spain, Portugal and Greece. It has become a problem as a forest pest insect because of feeding damage to trees such as pine and cedar. In addition, poisonous hair of the larva of this moth is known to cause a serious allergic reaction in humans, livestock, pets and the like. Moreover, in recent years, the habitat of the moth has been expanding northward from the Mediterranean region due to the effect of global warming. There is therefore a ...

METHOD FOR PRODUCING 2-CHLOROMETHYLBENZALDEHYDE, 2-CHLOROMETHYLBENZALDEHYDE-CONTAINING COMPOSITION, AND METHOD FOR STORING SAME

A process for obtaining an industrially useful 2-chloromethylbenzaldehyde-containing liquid composition at a high yield is provided. More specifically, a process for producing 2-chloromethylbenzaldehyde comprising step (A) of mixing 1-dichloromethyl-2-chloromethylbenzene and sulfuric acid having a concentration of 84.5% by weight or more; and step (B) of mixing a mixture obtained in step (A) and water is provided. 1. A process for producing 2-chloromethylbenzaldehyde comprising:step (A) of mixing 1-dichloromethyl-2-chloromethylbenzene and sulfuric acid having a concentration of 84.5% by weight or more; andstep (B) of mixing a mixture obtained in step (A) and water.2. The process according to claim 1 , comprising a step of neutralizing an organic phase of the mixture obtained in step (B).3. The process according to claim 1 , further comprising a step of mixing the resulting 2-chloromethylbenzaldehyde with at least one selected from the group consisting of a polymerization inhibitor and an antioxidant.4. The process according to claim 3 , wherein the at least one selected from the group consisting of a polymerization inhibitor and an antioxidant is at least one selected from the group consisting of 2 claim 3 ,6-bis(1 claim 3 ,1-dimethylethyl)-4-methylphenol(BHT) claim 3 , hydroquinone claim 3 , monomethyl hydroquinone and phenothiazine.5. The process according to claim 1 , wherein sulfuric acid having a concentration of 84.5% by weight or more in step (A) contains water at 0.4 mol or more based on 1 mol of 1-dichloromethyl-2-chloromethylbenzene.6. A composition comprising 2-chloromethylbenzaldehyde and at least one selected from the group consisting of a polymerization inhibitor and an antioxidant.7. The composition according to claim 6 , wherein the at least one selected from the group consisting of a polymerization inhibitor and an antioxidant is at least one selected from the group consisting of 2 claim 6 ,6-bis(1 claim 6 ,1-dimethylethyl)-4-methylphenol (BHT) ...

SYNTHETIC NAVEL ORANGEWORM PHEROMONE COMPOSITION AND METHODS RELATING TO PRODUCTION OF SAME

One or more embodiments of the invention are directed to the synthetic methods for making lepidopteran pheromones including navel orangeworm pheromones. The synthetic methods involve novel, efficient, and environmentally benign steps and procedures. 1. (canceled)4. The method of claim 2 , wherein said oxidation reaction of step A is an TEMPO oxidation.5. The method of claim 2 , wherein said alkylation reaction of step B is an O-Alkyl-C-alkoxy addition reaction.6. The method of claim 2 , wherein said reduction reaction and said hydrolysis reaction of step F is an alkyne reduction and an acetal hydrolysis.7. The method of claim 2 , further comprising:{'sup': 9', '6', '9, 'claim-text': {'sup': '9', 'Ris alkyl.'}, 'wherein, 'producing a compound of formula (8b) in step G, wherein step G comprises reaction of a compound of formula R—R—R(8a),'}8. The method of claim 7 , wherein Ris —CH.9. The method of claim 2 , wherein step H comprises a nucleophilic addition reaction.10. The method of claim 2 , wherein (8b) is synthesized from a compound of the formula R—R—R(8a) through an isomerization reaction.13. The method of claim 10 , wherein said alkylation reaction of step C is an alkynyl-de-halogenation reaction.14. The method of claim 10 , wherein step E is a cycle of oxidative additions and reductive eliminations.15. The method of claim 10 , wherein step E is a Cadiot-Chodkiewicz reaction.16. The method of claim 10 , wherein (5b) is 1-bromobut-1-yne.17. The method of claim 10 , wherein (5b) is synthesized from a compound of the formula R—R(5a) through a halogenation reaction claim 10 , wherein Ris —C≡CH.1830. The method of claim claim 10 , wherein (5a) is but-1-yne.19. The method of claim 10 , wherein (4) is a dialkoxy substituted alkynyl.20. The method of claim 10 , wherein (4) is 12 claim 10 ,12-diethoxydodec-1-yne. This application is a continuation of U.S. patent application Ser. No. 13/680,973 filed on Nov. 29, 2012, which in turn is a continuation of U.S. patent ...

7-METHYL-3-METHYLENE-7-OCTENAL ACETAL COMPOUND AND METHODS FOR PRODUCING ALDEHYDE COMPOUND AND ESTER COMPOUND USING THE SAME

There are provided methods of efficiently producing compounds that are, for example, sex pheromones of San Jose Scale. For example, there is provided a method for producing a 7-methyl-3-methylene-7-octenyl carboxylate compound (1), the method including the step of coupling a nucleophilic reagent expressed as a 3-methyl-3-butenyl M of General Formula (8): The following application is a divisional application of U.S. Non-Provisional application Ser. No. 16/788,808 filed Feb. 12, 2020, which is a divisional application of U.S. Non-Provisional application Ser. No. 15/825,299 filed Nov. 29, 2017, now U.S. Pat. No. 10,611,718, which are incorporated herein by reference in their entireties.The invention relates to a 7-methyl-3-methylene-7-octenal acetal compound and methods for producing an aldehyde compound and an ester compound using the acetal compound.3,7-Dimethyl-2,7-octadienal and a corresponding alcohol, 3,7-dimethyl-2,7-octadienol are widely applied as floral perfumes and fruit flavors. Their regioisomers having double bonds at different positions, 7-methyl-3-methylene-7-octenal and 7-methyl-3-methylene-7-octenol, are expected to be applied in the same fields. Stoyanova et al. have reported that 7-methyl-3-methylene-7-octenal exists in the essential oil of seeds of Amomum tsaoko (Godoshnik na Visshiya Khimikotekhnologicheski Institut, Sofiya, 31, 203 (1991), CODEN: GVKIAH, ISSN: 0489-6211).(generic name: San Jose Scale, hereinafter abbreviated as “SJS”) is widely distributed in the world, damages fruit trees and ornamental trees, especially deciduous fruit trees, and thus is an economically critical insect pest. Gieselmann et al. and Anderson et al. have found that the sex pheromone of SJS contains three active components of 7-methyl-3-methylene-7-octenyl propionate, (Z)-3,7-dimethyl-2,7-octadienyl propionate, and (E)-3,7-dimethyl-2,7-octadienyl propionate (Gieselmann et al., J. Chem. Ecol., 5, 891 (1979), Anderson et al., J. Chem. Ecol., 5, 919 (1979), and ...

Process for synthesizing GGA and its derivatives

This invention relates to processes for synthesizing GGA or GGA derivatives and intermediates involved therein. 7. The process of claim 1 , wherein R-Rare methyl.8. The process of claim 3 , wherein Ris methyl. This invention relates generally to geranylgeranyl acetone (GGA) or GGA derivatives and processes for their syntheses.Geranylgeranylacetone (GGA) is an acyclic isoprenoid compound with a retinoid skeleton having the formula:GGA is a known anti-ulcer drug used commercially and is reported to have neuroprotective and related effects. See, for example, PCT Pat. App. Pub. No. WO 2012/031028 and PCT Pat. App. No. PCT/US2012/027147, each of which is incorporated herein by reference in its entirety. Alternate methods for synthesizing GGA are provided herein.In various aspects, provided herein are processes of syntheses of GGA and derivatives thereof, and intermediates thereto.In one aspect, a process for preparing a compound of formula (I) is provided,said process comprising: hydrolyzing a compound of formula (II):wherein: X and Y are each independently OR, SR, or X and Y together with the carbon atom they are attached to form a ring of formula:wherein each Ris independently C-Calkyl, each Xand Xare independently O, or S; q is 1 or 2; each Xis independently C-Calkyl; t is 0, 1, 2, or 3, and each of R, R, R, R, and Ris independently H or C-Calkyl or Rand Rtogether with the carbon atom they are joined to form a C-Ccycloalkyl optionally substituted with 1-3 C-Calkyl.In further aspects, a process for preparing a compound of formula (II) is provided:said process comprising: contacting a compound of formula (III):wherein: the variables are defined as in formula (II) above with a compound of formula:wherein L is P(R), P(O)(R), SOR, Si(R), preferably P(R); and wherein is Ris a C-Calkyl group or an aryl group; under conditions suitable for olefination of compound of formula (III) to produce a compound of formula (II).In further aspects, a process for preparing a compound of ...

SYNTHESIS OF INTERMEDIATE FOR TREPROSTINIL PRODUCTION

The compound according to Formula I is an intermediate in the synthesis of prostacylin analogs. The present invention provides an efficient method for synthesizing a Formula I compound. 2. The improvement of claim 1 , wherein R claim 1 , Rand Rare each independently (C-C)alkyl.3. The improvement of claim 2 , wherein R claim 2 , Rand Rare each methyl.4. The improvement of claim 1 , wherein Ris (C-C)alkyl and Rand Rare each independently (C-C)cycloalkyl.5. The improvement of claim 1 , wherein integer x is 2.6. The improvement of claim 1 , wherein R is straight or branched (C-C)alkyl.7. The improvement of claim 1 , wherein R is methyl.8. The improvement of claim 1 , wherein R is (C-C)aryl(C-C)alkylene-.9. The improvement of claim 1 , wherein R is benzyl.10. The improvement of claim 1 , wherein the organolithium is phenyllithium claim 1 , or butyllithium.11. The improvement of claim 1 , wherein said hydrolyzing comprises contacting the compound of Formula A with an agent selected from the group consisting of water claim 1 , aqueous mineral acid claim 1 , and an aqueous solution of sodium sulfite.12. The improvement of claim 1 , wherein said hydrolyzing comprises contacting the compound of Formula A with an aqueous solution of sodium sulfite.13. The improvement of claim 1 , wherein the prostacyclin is treprostinil.15. The improvement of claim 14 , wherein said organolithium is phenyllithium.16. The improvement of claim 14 , wherein integer x is 1 and R claim 14 , Rand Rare methyl and wherein the allyl halide is allyl iodide.17. The improvement of claim 14 , wherein the prostacyclin is treprostinil.19. The compound of claim 18 , wherein R claim 18 , Rand Rare each independently (C-C)alkyl.20. The compound of claim 19 , wherein R claim 19 , Rand Rare each methyl.21. The compound of claim 20 , wherein Ris (C-C)alkyl and Rand Rare each independently (C-C)cycloalkyl.22. The compound of claim 18 , wherein integer x is 2.23. The compound of claim 18 , wherein R is straight or ...

METHODS FOR PRODUCING BETA-CYCLOLAVANDULAL AND DERIVATIVE OF SAME

Target compounds are synthesized simply, efficiently and selectively. More specifically, provided are a method for producing (2,4,4-trimethyl-1-cyclohexene)carbaldehyde, comprising the steps of: reacting the carbonyl group of 2,4,4-trimethyl-2-cyclohexenone (1) to obtain a 2,4,4-trimethyl-2-cyclohexenylidenemethyl ether compound (2) and hydrolyzing Compound (2) to obtain the (2,4,4-trimethyl-1-cyclohexene)carbaldehyde (3); a method for producing (2,4,4-trimethyl-1-cyclohexene)methanol, comprising a step of reducing Compound (3) to obtain the (2,4,4-trimethyl-1-cyclohexene)methanol (4); and a method for producing a (2,4,4-trimethyl-1-cyclohexenyl)methyl ester compound, comprising a step of esterifying Compound (4) to obtain the (2,4,4-trimethyl-1-cyclohexenyOmethyl ester compound (5). The present invention relates to methods for producing a monoterpene aldehyde, an alcohol and derivatives thereof that are important as biologically active substances or synthetic intermediates thereof. More specifically, the present invention relates to methods for producing (2,4,4-trimethyl-1-cyclohexene)carbaldehyde known as a general name of β-cyclolavandulal, (2,4,4-trimethyl-1-cyclohexene)methanol known as a general name of β-cyclolavandulol, and a (2,4,4-trimethyl-1-cyclohexenyl)methyl ester compound derived from the alcohol compound.(2,4,4-trimethyl-1-cyclohexene)carbaldehyde (β-cyclolavandulal) has been isolated from caraway, Carum carvi Linn., grown in India and used as a folk medicine and from fungi as a secondary metabolite (Non-Patent Document 1).The (2,4,4-trimethyl-1-cyclohexene)carbaldehyde (β-cyclolavandulal) is also known as a constituent of WS-9659A (lavanducyanine) and WS-9659B, which have been isolated from actinomycete Streptomyces as inhibitors of testosterone 5α-reductase (Non-Patent Document 2).Vellutini et al. have isolated a total of eight compounds including (2,4,4-trimethyl-1-cyclohexenyl)methyl esters (general name: β-cyclolavandulyl esters) and 4,4,6- ...

OMEGA-HALO-2-ALKYNAL, METHOD FOR PRODUCING SAME, AND METHOD FOR PRODUCING CONJUGATED Z-ALKEN-YN-YL ACETATE USING SAME

Provided is a method for industrially producing a conjugated Z-alken-yn-yl acetate such as Z-13-hexadecen-11-yn-yl acetate which is a sex pheromone component of a pine processionary moth, and an intermediate for the conjugated Z-alken-yn-yl acetate under mild conditions at a high yield. More specifically, provided is a method for producing a conjugated Z-alken-yn-yl acetate (5) comprising the steps of: reacting an ω-halo-2-alkynal (1) with an alkylidene triphenylphosphorane (3) through a Wittig reaction to obtain a conjugated Z-alken-yn-yl halide (4), and acetoxylating the conjugated Z-alken-yn-yl halide (4) into a conjugated Z-alken-yn-yl acetate (5). 3. The method for producing a conjugated Z-alken-yn-yl acetate according to claim 2 , wherein the conjugated Z-alken-yn-yl acetate is Z-13-hexadecen-11-yn-yl acetate. This application claims priority from Japanese Patent Application No. 2013-083861, filed Apr. 12, 2013, the disclosure of which is incorporated by reference herein in its entirety.The present invention relates to methods for producing a conjugated Z-alken-yn-yl acetate and an ω-halo-2-alkynal which is an intermediate thereof, particularly to a method for producing Z-13-hexadecen-11-yn-yl acetate which is a sex pheromone component of a pine processionary moth (scientific name: ), which is a forest pest insect in Europe.A pine processionary moth (scientific name: ) is an insect widely inhabiting European countries such as France, Italy, Spain, Portugal and Greece. It has become a problem as a forest pest insect because of feeding damage to trees such as pine and cedar. In addition, poisonous hair of the larva of this moth is known to cause a serious allergic reaction in humans, livestock, pets and the like. Moreover, in recent years, the habitat of the moth has been expanding northward from the Mediterranean region due to the effect of global warming. There is therefore a demand for the development of a novel control method of the moth.It has been reported ...

Directed Beta-C(sp3)–H Iodination and Arylation of Ketones

This invention discloses the first example of palladium(II)-catalyzed β-C(sp)-H iodination or arylation of a wide range of ketones by using a commercially available aminooxyacetic acid auxiliary. This L, X-type directing group overcomes the limitation of the transient directing group approach for -βC(sp)-H functionalization of ketones. Practical advantages of this method include simple installation of the auxiliary without chromatography, exceptional tolerance of a-functional groups, double bonds and triple bonds and rapid access to diverse sterically hindered quaternary centers. 1. A method of β-C(sp)-H iodination of a ketone having a β-hydrogen substituent , comprising:contacting the ketone and an aminooxyacetic acid in pyridine solvent to provide the corresponding oxime;then,contacting the oxime with iodine in the presence of a palladium(II) salt and phenyliodoniumacetate, in an aprotic solvent; then,{'sup': '3', 'hydrolyzing the oxime group under acidic conditions to provide the product β-C(sp)-iodoketone.'}2. The method of wherein the aminooxyacetic acid is aminooxyacetic acid or 2 claim 1 ,2-dimethylaminooxyacetic acid.3. The method of wherein the palladium(II) salt is palladium(II) acetate or palladium(II)trifluoroacetate.4. The method of wherein the aprotic solvent is dioxane or 1 claim 1 ,1 claim 1 ,1 claim 1 ,3 claim 1 ,3 claim 1 ,3-hexafluoroisopropanol.5. The method of wherein the oxime group is hydrolyzed in a solution of concentrated hydrochloric acid in dioxane.6. A method of β-C(sp)-H arylation of a ketone having a β-hydrogen substituent claim 1 , comprising:contacting the ketone and an aminooxyacetic acid in pyridine solvent to provide the corresponding oxime;then,contacting the oxime with an aryl iodide and silver trifluoroacetate in the presence of a palladium(II) salt, in an aprotic solvent; then,{'sup': '3', 'hydrolyzing the oxime group under acidic conditions to provide the product β-C(sp)-arylketone.'}7. The method of wherein the ...

Method for synthesizing 2,7-dimethyl-2,4,6-octatriene-1,8-dialdehyde

Provided in the present invention is a method for synthesizing 2,7-dimethyl-2,4,6-octatriene-1,8-dialdehyde. The synthesis method comprises the following steps: (1) adding acetaldehyde diethyl acetal and ethyl-(1-propenyl)-ether under the effect of a catalyst to produce 1,1,3-triethoxy-2-methyl-butane; (2) pyrolysis synthesizing 1,1,3-triethoxy-2-methyl-butane under the catalytic effects of isoquinoline and p-Toluenesulfonic acid to produce 1-methoxy-2-methyl-1,3-butadiene; (3) dissolving 1-methoxy-2-methyl-1,3-butadiene in anhydrous ethanol solvent for synthesis with a phase transfer catalyst, cetyl-trimethyl ammonium bromide, and a chlorinating agent, trichloroisocyanuric acid, to generate 4,4-diethoxy-3-methyl-1-chloro-butene; (4) combining 4,4-diethoxy-3-methyl-1-chloro-butene with a triphenylphosphine salt to produce a phosphonium salt; and (5) condensing the phosphonium salt under the effects of hydrogen peroxide in conjunction with sodium carbonate solution to generate 1,1,8,8-tetramethyl-2,7-dimethyl-2,4,6-octatriene; then hydrolyzing under acidic conditions to synthesize 2,7-dimethyl-2,4,6-octatriene-1,8-dialdehyde. The present invention has a simple process route, is easy to operate, and has mild conditions, great yield, and great industrial value.

METHOD FOR PREPARING 1-(4-CHLOROPHENYL)-2-CYCLOPROPYL-1-PROPANONE AND INTERMEDIATE THEREOF

A method is for preparing 1-(4-chlorophenyl)-2-cyclopropyl-1-propanone and an intermediate thereof, where in the method for preparing a compound of formula (I), α-alkoxy p-chlorobenzyl phosphonate (II) and cyclopropyl methyl ketone are used as raw materials, and subjected to a Homer-Wadsworth-Emmons reaction in an organic solvent in the presence of a base, so as to prepare a derivative of alkoxy propylene with the structure of formula (III); and the resulting derivative of alkoxy propylene (III) is hydrolyzed under acidic conditions to obtain 1-(4-chlorophenyl)-2-cyclopropyl-1-propanone (I). 2. The method according to claim 1 , wherein Ris methyl or ethyl.3. The method according to claim 1 , wherein the base is selected from sodium amide claim 1 , sodium hydride claim 1 , lithium diisopropylamide claim 1 , sodium methoxide claim 1 , sodium ethoxide claim 1 , sodium iso-propoxide claim 1 , sodium iso-butoxide claim 1 , potassium iso-butoxide claim 1 , sodium tert-butoxide claim 1 , or potassium tert-butoxide; and is preferably sodium amide claim 1 , sodium tert-butoxide or potassium tert-butoxide.4. The method according to claim 1 , wherein a reaction solvent for preparing the derivative of alkoxy propylene shown as formula (III) is selected from one or more of polar solvents such as methanol claim 1 , ethanol claim 1 , 1-propanol claim 1 , isopropanol claim 1 , 1-butanol claim 1 , isobutanol claim 1 , tert-butanol claim 1 , dimethyl formamide claim 1 , dimethyl acetamide claim 1 , N-methyl-pyrrolidone claim 1 , dimethyl sulfoxide claim 1 , dioxane and tetrahydrofuran claim 1 , or a mixture of one or more of the aforementioned polar solvents and a non-polar solvent such as benzene claim 1 , toluene claim 1 , dichloromethane or dichloroethane.5. The method according to claim 1 , wherein claim 1 , in the reaction for preparing the derivative of alkoxy propylene shown as formula (III) claim 1 , the molar ratio of α-alkoxy p-chlorobenzyl phosphonate (II) claim 1 , ...

1-HALO-6,9-PENTADECADIENE AND METHOD FOR PRODUCING (7Z,10Z)-7,10-HEXADECADIENAL

Provided are a 1-halo-6,9-pentadecadiene useful as an intermediate having a skipped diene skeleton and a method for producing (7Z,10Z)-7,10-hexadecadienal. More specifically, provided are a method for producing (7Z,10Z)-7,10-hexadecadienal including steps of subjecting a Grignard reagent formed from a (6Z,9Z)-1-halo-6,9-pentadecadiene to a nucleophilic substitution reaction with an orthoformate ester to obtain a (7Z,10Z)-1,1-dialkoxy-7,10-hexadecadiene; and hydrolyzing the (7Z,10Z)-1,1-dialkoxy-7,10-hexadecadiene in the absence of an oxidation reaction to obtain the (7Z,10Z)-7,10-hexadecadienal; and the like. 3. The method for producing (7Z claim 2 ,10Z)-7 claim 2 ,10-hexadecadienal according to claim 2 , further comprising a step of treating a 3-nonyltriarylphosphonium halide with a metal alkoxide of an alcohol having a pKa of from 12.0 to 16.5 at a temperature of from −20 to 0° C. to obtain the triarylphosphonium (3Z)-3-nonylide (4-3Z).4. A 1-halo-6 claim 2 ,9-pentadecadiene of Formula (1):{'br': None, 'sub': 3', '2', '4', '2', '2', '5, 'CH(CH)CH═CHCHCH═CH(CH)X\u2003\u2003(1),'}wherein X stands for a halogen atom.6. The method for producing a (6Z claim 5 ,9Z)-1-halo-6 claim 5 ,9-pentadecadiene according to claim 5 , further comprising a step of treating a 3-nonyltriarylphosphonium halide with a metal alkoxide of an alcohol having a pKa of from 12.0 to 16.5 at a temperature of from −20 to 0° C. to obtain the triarylphosphonium (3Z)-3-nonylide (4-3Z). The invention relates to a 1-halo-6,9-pentadecadiene and a method for producing (7Z,10Z)-7,10-hexadecadienal.An organic compound having a skipped diene skeleton such as a structure having two double bonds bonded via a single methylene carbon, in particular, an organic compound having a Z,Z-skipped diene skeleton is abundant in natural products such as polyunsaturated fatty acids, bioactive substances and pheromones so that an intermediates having a skipped diene skeleton is very useful.Chilean carpenter moth () is ...

METHOD FOR PRODUCING ALDEHYDE COMPOUND, AND ACETAL COMPOUND

Provided are a method for producing 3-methylglutaraldehyde in a good yield under a mild condition and a novel acetal compound which is useful for carrying out the foregoing method. The method is a production method of 3-methylglutaraldehyde including a step of hydrolyzing a compound represented by the following general formula (1): The present invention relates a production method of 3-methylglutaraldehyde an a acetal compound.3-Methylglutaraldehyde 3-methyl-1,5-pentanedial, hereinafter abbreviated as “MGL”) is a useful compound as a curing gent for photosensitive material, a tanning agent or leather, and a synthesis intermediate (see, for example, PTLs 1 to 3). As a production method of MGL, a method of hydrolyzing pyranyl ether which is obtained by the Diels-Alder reaction between croton aldehyde and methyl vinyl ether is known (see NPLs 1 and 2).PTL 1: JP 07-281342 APTL 2: DE 2137603 APTL 3: JP 2600-10224NPL 1: , Vol. 34, p.29 (1954)NPL 2: , Vol. 34, p.71 (1954)According to the aforementioned conventional methods, the reactivity of the Diels-Alder reaction between croton aldehyde and methyl vinyl ether is low, a severe condition of high temperature and high pressure is required, and the yield of MGL is low. Thus, there was room for improvement. In consequence, an object of the present invention is to provide a method for producing MGL in a good yield under a mild condition and a novel acetal compound which is useful for carrying out the foregoing method.In accordance with the present invention, the aforementioned object is achieved by the following [1] to [3].wherein Rand Reach independently represent an alkyl group having 1 to 6 carbon atoms, or are mutually coupled to represent an alkylene group having 2 to 6 carbon atoms.,wherein Rand Reach independently represent an alkyl group having 1 to 6 carbon atoms, or are mutually coupled to represent an alkylene group having 2 to 6 carbon atoms, to hydroformylation to obtain the acetal compound (1).wherein Rrepresents ...

2,7-二甲基-2,4,6-辛三烯-1,8-二醛的合成方法

本发明提供了2，7-二甲基-2，4，6-辛三烯-1，8-二醛的合成方法，所述合成方法包括如下步骤：(1)乙醛二乙基乙缩醛与乙基(1-丙烯基)醚在催化剂的作用下加成得到1，1，3-三乙氧基-2-甲基-丁烷；(2)1，1，3-三乙氧基-2-甲基-丁烷在异喹啉和对甲苯磺酸催化作用下裂解合成得到1-甲氧基-2-甲基-1，3-丁二烯；(3)1-甲氧基-2-甲基-1，3-丁二烯溶在无水乙醇溶剂中与相转移催化剂十六烷基三甲基溴化铵和氯化试剂三氯异氰尿酸合成生成4，4-二乙氧基-3-甲基-1-氯丁烯；(4)4，4-二乙氧基-3-甲基-1-氯丁烯与三苯基膦成盐合成得到膦盐；和(5)膦盐在双氧水作用下并用碳酸钠溶液缩合生成1，1，8，8-四甲基-2，7-二甲基-2，4，6-辛三烯；再在酸性条件下水解合成2，7-二甲基-2，4，6-辛三烯-1，8-二醛。本发明的工艺路线简捷，操作简单，条件温和，收率良好，极具工业价值。

Improved process for preparing hydrazine hydrate with pyrazoline recycling

본 발명은 활성제의 존재 하에서 암모니아를 과산화수소로 산화시킴으로써 메틸 에틸 케톤으로부터 얻어진 메틸 에틸 케톤의 아진으로부터 하이드라진 수화물을 제조하는 개선된 공정으로서, 피라졸린-클래스 헤테로사이클 퍼지를 재순환시키는 단계를 포함함을 특징으로 하는 개선된 공정에 관한 것이다.

A kind of method of synthesis 3,3- dimethyl butyraldehydes

本发明提供一种制备3,3‑二甲基丁醛的工艺方法，在容器中，氮气保护，加入有机溶剂和固体酸催化剂，滴加叔丁基氯，再滴加烷基酸类乙烯酯，保温反应后过滤除去催化剂，将有机层减压蒸馏，再加入碱或者酸加热回流水解得粗品，粗品再精馏得3,3‑二甲基丁醛成品。本发明原料成本低，反应条件温和，操作简单副反应少，安全环保，利与工业化生产。

Preparation of certain benzodiazepine compounds

Method for producing alkoxymethylbenzaldehyde

The manufacture method of 2 ' trifluoromethyl substituted aroma race ketone

本发明涉及一种2’‑三氟甲基取代芳香族酮的制造方法，使2‑卤代三氟甲苯化合物与镁金属反应而转化成格利雅试剂，使该格利雅试剂与酸酐反应，然后进行水解处理，制造2’‑三氟甲基取代芳香族酮。本发明的2’‑三氟甲基取代芳香族酮的制造方法不使用高价的原料，将格利雅试剂作为中间体生成，使该格利雅试剂与酸酐有效地反应，由此可以制造2’‑三氟甲基取代芳香族酮。通过本发明的2’‑三氟甲基取代芳香族酮的制造方法制造的2’‑三氟甲基取代芳香族酮可以用作精密化学、医农药原料、树脂/塑料原料、电子信息材料、光学材料等。

Method for producing deoxybenzoin

本発明はアリールアセトニトリルを芳香族化合物と反応させることおよびその生成したケチミン化合物を加水分解することにより1,2-ジアリールエタノンを製造する方法であって、反応に用いる溶媒は、少なくとも1種のモノアルキレングリコール若しくはポリアルキレングリコールのジアルキルエーテル又は少なくとも2個の酸素原子を有する環状エーテルである、上記方法に関する。この方法は室温で卓越した収率を与え、溶媒は無水である必要はない。

IMPROVED PROCESS FOR THE PREPARATION OF HYDRAZINE HYDRATE WITH PYRAZOLINE RECYCLING

La présente invention concerne un procédé amélioré de préparation d'hydrate d'hydrazine à partir de l’azine de la méthyl éthyl cétone obtenue à partir de la méthyl éthyl cétone par oxydation de l'ammoniac par l'eau oxygénée en présence d'un activateur, caractérisé en ce qu’il comprend une étape de recyclage de la purge des hétérocycles de la famille de la pyrazoline. The present invention relates to an improved process for the preparation of hydrazine hydrate from the azine of methyl ethyl ketone obtained from methyl ethyl ketone by oxidation of ammonia with hydrogen peroxide in the presence of a activator, characterized in that it comprises a step of recycling the purge of the heterocycles of the pyrazoline family.

PROCESS FOR THE PREPARATION OF 4-ARYL-1-TETRALONES

5-Chloro-5-substd.-2-norbornenes prodn - by reacting cyclopentadiene lanthanide salt with an alkylating agent and then with a chlorovinyl cpd.

Norbornenes of formula (I): (R=1-6C alkyl; 2-4C alkenyl, 5-9C cycloalkyl, opt. substd. by alkyl, benzyl, phenethyl, phenylpropyl, furfuryl 2-8C alkoxymethyl or benzyloxymethyl, X=cyano, COOH, halocarbonyl, formul or alkoxycarbonyl; R1=H,CH3 or phenyl) are prepd by reacting RY, (Y=halo or ZSO2.O; Z=lower alkyl, phenyl, tolyl or halophenyl) with an organometallic cpd. formed from a lanthanide metal and cyclopentadiene, then reacting with R'.CH=C(Cl)X. (I) are intermediates in the total synthesis of prostaflandins and related cpds. Intermetallic cpd is non-toxic and reacts quickly (>=1hr) giving a nearly theoretical yield of the desired isomer.

PROCESS FOR THE PREPARATION OF HYDRAZINE HYDRATE

IMPROVED PROCESS FOR THE PREPARATION OF HYDRAZINE HYDRATE WITH PYRAZOLINE RECYCLING

La présente invention concerne un procédé amélioré de préparation d'hydrate d'hydrazine à partir de l’azine de la méthyl éthyl cétone obtenue à partir de la méthyl éthyl cétone par oxydation de l'ammoniac par l'eau oxygénée en présence d'un activateur, caractérisé en ce qu’il comprend une étape de recyclage de la purge des hétérocycles de la famille de la pyrazoline. The present invention relates to an improved process for the preparation of hydrazine hydrate from the azine of methyl ethyl ketone obtained from methyl ethyl ketone by oxidation of ammonia with hydrogen peroxide in the presence of a activator, characterized in that it comprises a step of recycling the purge of the heterocycles of the pyrazoline family.

Process for preparing alpha-ketoaldehydes

Hydroxydihydrocitronellal ethers and acetals - prepd from citronellal by reaction with amines and then alcohols

Ethers of hydroxydihydrocitronellal, and its homologues, of formula RO-C(CH3)2-CH2-CH2-CH2-CH(CH3)-CH2-CHO (I) (where R is 1-4C alkyl, esp. Me or Et) are prepd. in good yield and sufficient purity for direct use in perfumery, by reacting citronellal or its homologues with a prim. or sec. amine or NH3, esp. at -10 to +40 degrees C; contacting the prod. with an alcohol ROH in the presence of a strong acid, esp. in at least equimolar concns.; neutralising the reaction compsn. with an alkaline reagent and sepg. (I) and pref. any acetal by-prod., pref. of formula RO-C(CH3)2-CH2-CH2-CH2-CH(CH3)-CH2-CH)OR)2 (II), esp. where R is Me. (II), which have a pleasant smell, are useful in perfumery or in insecticidal compsns.

PROCESS FOR THE PREPARATION OF HALOGENOMETHYL DIPHENYL ETHERS

Procédé de préparation d'éthers diphényliques m-halogénométhylés de formule : Process for the preparation of m-halogenomethylated diphenyl ethers of the formula:

Patent FR2202869B2

Patent FR2381014B1

Process for the production of cycloalkanones

Polyalkylindanes and products derived therefrom as well as process for the manufacture of said

Process for preparing carvone from limonene

Preparation method of 3,3,3-trifluoropropionaldehyde

本发明公开了一种3，3，3-三氟丙醛的制备方法，该方法在三口烧瓶中加入1，1-二烷氧基-3，3，3-三氟丙烷(CF 3 CH 2 CH(OR) 2 )、乙酸和催化剂，升温至90℃～140℃，搅拌下反应2h～8h。其中1，1-二烷氧基-3，3，3-三氟丙烷CF 3 CH 2 CH(OR) 2 中R为CH 3 ，C 2 H 5 C 3 H 7 ，C 4 H 9 ，C 5 H 11 ，C 6 H 13 ，C 7 H 15 ，C 8 H 17 ，C 9 H 19 ，C 10 H 21 ；所用催化剂为硫酸、盐酸、对甲苯磺酸、甲基磺酸、三氟乙酸；其中1，1-二烷氧基-3，3，3-三氟丙烷：乙酸：催化剂的摩尔比为1：2～2.5：0.1～0.6。

Process for the preparation of 4- (disubstituted phenyl) -1-tetralones

Preparation of hydrazine hydrate

Preparation of hydrazine hydrate by hydrolysis of methyl ethyl ketone azine involves purging pyrazoline heterocycles sufficiently to avoid coloration of the hydrazine hydrate product.

Synthetic method for licochalcone C

본 발명자들은 Al 2 O 3 를 이용한 C -프레닐화 방법, 위치선택적 보호기화 및 메틸화, 그 이후에 염기 조건 하에서 통상적인 클라이젠-슈미트 응축반응을 수행하여 리코찰콘 C를 제조하였다. 물에 의해 촉진되는 [3,3]-시그마결합 자리옮김반응은 분해 문제로 인하여 리코찰콘 C 합성에 적용할 수 없었으나, 본 발명자들은 Al 2 O 3 를 이용한 위치선택적 C -프레닐화가 리코찰콘 C를 합성하는 새로운 방법임을 밝혔다. The present inventors have made a method of C -prernylation using Al 2 O 3 , position selective protection and methylation, followed by a conventional Clagen-Schmid condensation reaction under basic conditions to produce Ricochalcone C. Although the water-promoted [3,3] -sigma binding site transfer reaction could not be applied to the synthesis of Ricochalcone C due to degradation problems, the present inventors have found that positionally selective C -prenylation using Al 2 O 3 , C as a new method to synthesize.

Improved process for the production of synthetic japan or borneo camphor

Borneol is obtained by treating pinene hydrochloride with a hydroxide, e.g. calcium hydroxide, or with boiling water. Camphor is produced from pinene hydrochloride by simultaneous treatment with an oxidizing agent and a "dehydrogenizing" substance. Metallic oxides and peroxides, e.g. iron oxide and lead peroxide, are given as examples of oxidizing agents; bisulphates, e.g. potassium bisulphate, and bicarbonates are mentioned as "dehydrogenizing" substances. Camphor may also be produced by treating borneol with a peroxide or the like.

Method for producing deoxybenzoins

本发明涉及一种通过使芳基乙腈与芳族化合物反应并水解形成的酮亚胺化合物而制备1，2－二芳基乙酮的方法，其中用于该反应的溶剂为至少一种单－或多亚烷基二醇的二烷基醚或者具有至少两个氧原子的环醚。该方法在室温下的产率优异并且不需要干燥溶剂。

Method of preparing 2-hydroxy-3-alkyl-2-cyclopenten-1-one

A method of preparing 2-hydroxy-3-alkyl-2-cyclopenten-1-one which comprises reacting 2-alkyl-5-carboalkoxycyclopentanone with nitrite in the presence of water and alkali; rendering the reaction system acidic; and either treating the mass for hydrolysis by heating or carrying out oxime exchange reaction in the presence of an aliphatic lower carbonyl compound added as an acceptor to the acidified reaction system.

Muscone preparation process

Utilize the method that micro-structured reactor prepares cyclocitral

本发明是一种利用微结构反应器制备环柠檬醛的方法。其步骤是将液体原料柠檬醛与有机胺按摩尔比1:0.8～1.5同时泵入管式反应器或微结构反应器中进行胺化反应,反应器反应温度控制在‑10～20℃，控制反应液的流速使其在反应器中的总停留时间为0.1～25min,将得到的醛亚胺与浓硫酸注入另外一个微结构反应器中进行关环反应。反应产物经过氢氧化钠溶液中和，酸性水解，分液，减压蒸馏，干燥得到浅黄色油状产品环柠檬醛。本发明方法反应时间短，反应温度精准可控，产品选择性，收率高。本发明步骤简单、操作方便、实用性强。

Cyclohexanone oxime derivatives, process for their preparation and further processing to cyclohexanone derivatives

Process for preparation of hydrazine hydrate

本发明涉及生产水合肼的方法,其中水解甲基乙基酮吖嗪以获得水合肼及甲乙酮,其特征为,吡唑啉族的杂环化合物以足以防止水合肼着色的量除去。

METHOD FOR PRODUCING 4-ARYL DISUBSTITUTED-1-TETRALONES.

The present invention relates to a process for preparing a 1-disubstituted 4-aryltetralone of formula <IMAGE> in which X denotes halogen, C1-C4 alkyl or C1-C4 alkoxy, and Y, situated in position 2' or 3', denotes halogen or C1-C4 alkyl, this process being characterised in that it comprises the reaction, in the presence of an acidic agent, of alpha -naphthol of formula (II) with an aromatic hydrocarbon of formula (III) <IMAGE> where X denotes halogen, C1-C4 alkyl or C1-C4 alkoxy, and Y is situated in the ortho or meta position relative to X and denotes halogen or C1-C4 alkyl.

Preparation method of 2,6,11, 15-tetramethyl-2, 4,6,8,10,12, 14-hexadecaheptadien dialdehyde

本发明提供了一种2，6，11，15‑四甲基‑2，4，6，8，10，12，14‑十六碳七烯二醛的制备方法，所述制备方法包括如下步骤：(1)以1，2‑二卤代乙烷为原料，在催化剂作用下与亚磷酸三乙酯经Michaelis‑Arbuzov反应得到亚乙基二膦酸四乙酯；(2)该膦酸酯与丙酮醛缩二甲醇在碱作用下经Horner‑Wadsworth‑Emmons反应得到3‑甲基‑4，4‑二甲氧基‑2‑丁烯‑1‑膦酸二乙酯；(3)接着所述膦酸二乙酯不经分离直接与2，7‑二甲基‑2，4，6‑辛三烯‑1，8‑二醛反应“一锅法”得到2，6，11，15‑四甲基‑2，4，6，8，10，12，14‑十六碳七烯二醛缩四甲醇；(4)最后该缩醛化合物在酸性条件下水解脱保护得到目标化合物2，6，11，15‑四甲基‑2，4，6，8，10，12，14‑十六碳七烯二醛。本发明的“一锅法”工艺路线原料易得，简捷连贯，操作简单，条件温和，收率良好，三废较少，适于工业化生产。

Method for preparing hydrazine hydrate

The invention concerns a method for making hydrazine hydrate which consists in hydrolyzing methyl ethyl ketone azine to obtain hydrazine hydrate and methyl ethyl ketone, characterised in that it consists in purging heterocyclic compounds of the pyrazoline family to prevent coloration of the hydrazine hydrate.

1-methoxyl-2,6,10-trimethyl-1,3,5,9-undecene tetraene and preparation method and application thereof

本发明公开了一种中间体1-甲氧基-2，6，10-三甲基-1，3，5，9-十一碳四烯及其制备方法和应用。目前的番茄红素中间体2-位双键C-14醛(2，6，10-三甲基-2，5，9-十一烷三烯-1-醛)，其合成方法中要用到昂贵的碘甲烷、有污染的二甲硫醚和危险的强碱，较难应用于工业生产。本发明提供了一种新化合物1-甲氧基-2，6，10-三甲基-1，3，5，9-十一碳四烯，利用其进行水解、精制即可制得纯的2-位双键C-14醛，简化合成路线，适合工业生产。

Stop control circuit for brushless DC motor

A stop control circuit for a DC motor causes the motor to stop precisely by purely electrical action. A DC motor is provided with a bidirectional driving circuit, a servo circuit for controlling the driving circuit, and a rotation detector associated with the motor shaft to provide a phase signal that depends, in magnitude and polarity, on the particular rotational angle of the shaft, regardless whether the motor is turning. A stop control circuit then includes an amplifier whose output varies according to the phase signal, and a switch that normally provides the servo signal to the driving circuit, but, upon command, switches over to provide thereto the output of the amplifier as a brake signal. Alternatively the rotation detector can include two sensor elements separated by π/2, and the stop control circuit can include an inverting amplifier, a non-inverting amplifier coupled to one of the sensor elements, and a switch circuit with inputs coupled respectively to these amplifiers. A comparator provides a switch signal to the switch circuit in dependence on the phase signal from the other sensor element. In another embodiment, a differential amplifier provides a brake signal in dependence upon both the phase signals from the two sensor elements.

The technique that hydroxylamine hydrochloride is prepared using oxime acid hydrolysis method

本发明属于盐酸羟胺制备技术领域，公开了采用肟酸解方法制备盐酸羟胺的工艺，其包括如下步骤：步骤a）原料缓存配置工序，步骤b）酸解反应工序，步骤c）酮肟精馏工序，步骤d）脱水干燥工序，步骤e）乙醇回收工序，步骤f）乙醛肟化工序。本发明工艺优化了甲乙酮肟酸解生产盐酸羟胺的工艺路线及技术参数，应用了渗透汽化耦合技术，提高了产品收率和质量，促进了行业技术进一步提高，带动了相关产业的发展，同时实现了资源合理利用。

Method for purifying acetone from waste residue and waste water produced in ketene dimmer production process

本发明公开一种从双乙烯酮生产过程产生的废渣、废水中提纯丙酮的方法，所述废渣是指残渣稀释液，所述废水是指提浓废水，其特征在于，包括三大步骤，第一步，残渣稀释液和稀酸反应生成丙酮，第二步，从提浓废水中回收丙酮，第三步，将前两步得到的丙酮混合进行精馏提纯；采用本发明进行丙酮回收和提纯，不仅能够增加产量，而且含量显著提高了，大幅增加附加值，同时还可以回收以前外卖丙酮中的一部分醋酸，有效节约双乙烯酮的生产成本。

Improved process for preparing hydrazine hydrate with pyrazoline recycling

The present invention relates to an improved process for preparing hydrazine hydrate from the azine of methyl ethyl ketone obtained from methyl ethyl ketone by oxidizing ammonia with hydrogen peroxide in the presence of an activator, characterized in that it comprises a step of recycling the pyrazoline-class heterocycles purge.

The preparation method of isophorone

本发明涉及异佛尔酮的制备方法，该方法是通过作为进料物的丙酮的催化羟醛缩合、反应产物的后处理、有价值料流的水解和将其分离成有机级分和含水级分、从有机级分中获得异佛尔酮、将含水级分进行蒸馏后处理并将蒸馏后处理设备顶部的蒸气进一步输送到水解设备中而进行的。

METHOD FOR PREPARING DISSERSTITUTED 4-ARYL-1-TETRALONES

PROCESS FOR THE PREPARATION OF HALOGENOMETHYL DIPHENYL ETHERS

Preparation method of 3-bromo-4-hydroxybenzaldehyde

本发明公开了一种3‑溴‑4‑羟基苯甲醛的制备方法，包括以下步骤：(1)步骤(1)得到的对羟基苯甲缩醛与溴素进行溴化反应，得到3‑溴‑4‑羟基苯甲缩醛；(2)对步骤(1)得到的3‑溴‑4‑羟基苯甲缩醛进行水解反应，反应完全后经过后处理得到所述的3‑溴‑4‑羟基苯甲醛。该制备方法通过将醛替换为缩醛进行溴化反应，有效地避免了二溴代产物的生成，提高了一溴代产品的收率和纯度，更加便于工业化。

Method for synthesizing 2,7-dimethyl-2,4,6-octatriene-1,8-dialdehyde

Provided in the present invention is a method for synthesizing 2,7-dimethyl-2,4,6-octatriene-1,8-dialdehyde. The synthesis method comprises the following steps: (1) adding acetaldehyde diethyl acetal and ethyl-(1-propenyl)-ether under the effect of a catalyst to produce 1,1,3-triethoxy-2-methyl-butane; (2) pyrolysis synthesizing 1,1,3-triethoxy-2-methyl-butane under the catalytic effects of isoquinoline and p-Toluenesulfonic acid to produce 1-methoxy-2-methyl-1,3-butadiene; (3) dissolving 1-methoxy-2-methyl-1,3-butadiene in anhydrous ethanol solvent for synthesis with a phase transfer catalyst, cetyl-trimethyl ammonium bromide, and a chlorinating agent, trichloroisocyanuric acid, to generate 4,4-diethoxy-3-methyl-1-chloro-butene; (4) combining 4,4-diethoxy-3-methyl-1-chloro-butene with a triphenylphosphine salt to produce a phosphonium salt; and (5) condensing the phosphonium salt under the effects of hydrogen peroxide in conjunction with sodium carbonate solution to generate 1,1,8,8-tetramethyl-2,7-dimethyl-2,4,6-octatriene; then hydrolyzing under acidic conditions to synthesize 2,7-dimethyl-2,4,6-octatriene-1,8-dialdehyde. The present invention has a simple process route, is easy to operate, and has mild conditions, great yield, and great industrial value.

Process for the preparation of benzophenthiones and benzophenones

A process comprising the reaction of an optionally substituted benzene with thiophosgene in the presence of a Friedel Crafts catalyst for the preparation of the equivalent optionally substituted benzophenthione. The benzophenthiones are converted into the equivalent benzophenone derivatives by hydrolysis.

Process for producing optically active 3,7-dimethyl-6-octenol and process for producing intermediate therefor

Synthesis of the bicyclo[3.3.1]nonane structure

본 발명에 따르면, 알파,베타-불포화 알데히드 화합물에 대하여 2당량의 에틸 아세토아세테이트를 포타슘 t -부톡시드 염기 하에서 t -부탄올을 용매로 사용하여 가열하는 단일 조작에 의해 효율적으로 바이시클로[3.3.1]노난 구조 화합물을 제조하며, 상기 화합물의 염기 수용액(바람직하게는 1M NaOH) 조건에서의 가수분해에 의하여 3-케토-바이시클로[3.3.1]노난-1-올 구조 화합물을 제조하는 방법이 제공된다. 본 발명의 방법에 따르면, 값싸고 구입이 용이한 반응물질을 사용하여 경제적이며, 온화한 조건에서 반응이 진행되기 때문에 높은 수율로 다양한 치환체를 갖는 바이시클로[3.3.1]노난 화합물을 얻을 수 있다. According to the present invention, bicyclo [3.3.1 is efficiently carried out by a single operation of heating 2 equivalents of ethyl acetoacetate to alpha, beta-unsaturated aldehyde compound using t -butanol as a solvent under potassium t -butoxide base. ] Nonane structural compounds are prepared, and 3-keto-bicyclo [3.3.1] nonan-1-ol structural compounds are prepared by hydrolysis under basic aqueous solution of the compound (preferably 1M NaOH). Is provided. According to the method of the present invention, bicyclo [3.3.1] nonane compounds having various substituents can be obtained in high yield because the reaction proceeds under economical and mild conditions using inexpensive and easy to purchase reactants. 식 중, R은 수소 또는 카르보에톡시(CO 2 Et)를 나타내며, R 1 , R 2 은 각각 독립적으로 수소, 탄소수 1∼5의 저급 알킬 또는 탄소수 10 이하의 아릴로 이루어진 군으로부터 선택된다. In the formula, R represents hydrogen or carboethoxy (CO 2 Et), and R 1 and R 2 are each independently selected from the group consisting of hydrogen, lower alkyl having 1 to 5 carbon atoms or aryl having 10 or less carbon atoms.

Synthetic navel orangeworm pheromone composition and methods relating to production of same

本发明的一个或多个实施方案涉及用于制备鳞翅目昆虫信息素、包括脐橙螟信息素的合成方法。合成方法包括新的、有效的并且环境良性的步骤和程序。

METHOD FOR PRODUCING HYDRAZINE HYDRODATE

Method of producing 2′-trifluoromethyl group-substituted aromatic ketone

A method produces a 2′-trifluoromethyl-substituted aromatic ketone and includes reacting a 2-halogen-substituted benzotrifluoride compound with magnesium metal to convert the compound to a Grignard reagent; and reacting the Grignard reagent with an acid anhydride; and then hydrolyzing the resultant to produce a 2′-trifluoromethyl-substituted aromatic ketone. The method of producing a 2′-trifluoromethyl-substituted aromatic ketone enables 2′-trifluoromethyl-substituted aromatic ketone to be produced without using expensive raw materials by generating a Grignard reagent as an intermediate and reacting this Grignard reagent with an acid anhydride in an efficient productivity. The 2′-trifluoromethyl-substituted aromatic ketone that is produced by the method of producing a 2′-trifluoromethyl-substituted aromatic ketone can be used as fine chemicals, raw materials for pharmaceuticals and agrochemicals, raw materials for resins and plastics, electronics and information related materials, optical materials, and the like.

Chlorination of substituted alkenes using trichloroisocyanuric acid

Vinylether compounds, aldehyde compound, process for preparing the aldehyde compound and a carboxylate compound therefrom

The present invention provides a vinylether compound of the following general formula (1), wherein R 1 represents a monovalent hydrocarbon group having 1 to 15 carbon atoms, and the wavy line represents the E-form, the Z-form, or a mixture thereof. The present invention further provides a process for preparing 2,3,4,4-tetramethyl-1-cyclopentenecarbaldehyde of the following formula of the following formula (2), the process comprising subjecting the vinylether compound (1) to a hydrolysis reaction to form 2,3,4,4-tetramethyl-1-cyclopentenecarbaldehyde (2).

Preparation method of 2, 6-diethyl-4-methylphenylacetic acid

本发明涉及有机合成领域，尤其涉及一种唑啉草酯中间体(2,6‑二乙基‑4‑甲基)苯乙酸的合成方法，包括如下步骤：2,6‑二乙基‑4‑甲基苯胺通过Meerwein芳基化反应与醋酸乙烯酯反应生成1‑乙氧羰基‑1‑氯‑2‑（2,6‑二乙基‑4‑甲基苯基）乙烷；1‑乙氧羰基‑1‑氯‑2‑（2,6‑二乙基‑4‑甲基苯基）乙烷在酸性条件下水解生成2,6‑二乙基‑4‑甲基苯乙醛；2,6‑二乙基‑4‑甲基苯乙醛通过NaClO 2 氧化反应生成2,6‑二乙基‑4‑甲基苯乙酸。本发明优势在于避免了昂贵的贵金属催化剂和剧毒的氰化试剂的使用，所用试剂对环境友好，降低了成本，简化了工艺，收率较高，克服了现有技术的不足，适宜大规模工业化生产。

STOP CONTROL CIRCUIT FOR A DC MOTOR WITHOUT MANIFOLD

Process for the preparation of benzoyl chlorides and benzaldehydes

1341880 Acid chlorides and aldehydes ARGUS CHEMICAL CORP 19 April 1971 [16 March 1970] 24970/71 Headings C2C and C2P The invention comprises the reaction of a carboxylic acid with a benzopolychloromethane of the general formula wherein Ar is a benzene ring or two or more benzene rings either fused together or linked by C-C bonds as in diphenyl or by a bridging radical which is inert to the reaction conditions, R<SP>1</SP> is a hydrogen or halogen atom, an alkoxy or hydrocarbon group or a heterocyclic group containing one or more N, O or S heteroatoms, singly or in combination, or a hydrocarbon or such a heterocyclic group having at least one substituent inert to the reaction, n is 0 or 1 and m 2 is 1-6, in the presence of stannous or stannic chloride at 40-170‹ C. and the recovery of the acid chloride of the carboxylic acid and the acid chloride or aldehyde corresponding to the benzopolychloromethane of the general formula wherein X is H or Cl, from the reaction mixture. Tris - (2 - dichloromethylphenyl) phosphate is prepared by chlorination of tri-o-tolylphosphate.

Process for the production of cyclododecanone

Process for preparing halogenomethyldiphenyl ether and hydroxymethyldiphenyl ether

Preparation of ethers from citronellal or homologues thereof

7-Alkoxydihydrocitronellals (and their homologues) and their acetals useful as perfumes are prepared from citronellal (or homologues thereof) by reaction with ammonia or a primary or secondary amine, followed by treatment of the product with an alkanol in the presence of a strong acid and then neutralization of the reaction mixture.

Cyclohexanone-oxime derivatives, method for their preparation as well as method for their further processing into cyclohexanone- and cyclohexylamine derivatives

PROCEDURE FOR THE PREPARATION OF DEOXIBENZOINS

Se describe un procedimiento para la preparación de 1,2-diariletanonas por conversión de un arilacetonitrilo y un compuesto aromático e hidrólisis del compuesto de cetimina formado, en donde para la conversión se utiliza como solvente por lo menos un éter dialquílico de un mono o polialquilenglicol o un éter cíclico con por lo menos dos átomos de oxígeno. El procedimiento da buenos rendimientos a temperatura ambiente y no requiere un secado del solvente. A process for the preparation of 1,2-diarylethanones by conversion of an arylacetonitrile and an aromatic compound and hydrolysis of the ketimine compound formed is described, wherein at least one dialkyl ether of a mono or polyalkylene glycol is used as the solvent for conversion. or a cyclic ether with at least two oxygen atoms. The process gives good yields at room temperature and does not require solvent drying.

Preparation of 3,3-dimethylbutyraldehyde from a tert-butyl cation precursor, vinyl chloride and an acidic catalyst

This invention provides a method for preparing 3,3-dimethylbutyraldehyde from a tert-butyl cation precursor and vinyl chloride. The tert-butyl cation precursor is contacted with vinyl chloride in the presence of an inorganic acid, and the product is allowed to react with water to form 3,3-dimethylbutyraldehyde.

METHOD FOR PRODUCING AROMATIC ALDEHYDES

The synthesis technique of 1 (4 fluorophenyl) 2 (trans 4 alkyl-cyclohexyl) ethyl ketone

本发明公开了一种新的合成1‑(4‑氟苯基)‑2‑(反式‑4‑烷基环己基)‑乙酮的工艺路线，以反式‑4‑烷基‑1‑(羟甲基)环己烷为原料，先与取代磺酰氯反应生成中间体‑反式‑4‑烷基环己烷基‑1‑亚甲基的对甲苯磺酸酯，不经分离直接加入氰化钾取代苯磺酸根生成反式‑4‑烷基‑1‑(氰基甲基)环己烷，最后与对氟苯基格氏试剂反应，再经水解制备‑1‑(4‑氟苯基)‑2‑(反式‑4‑烷基环己基)‑乙酮。本发明具有工艺路线短、副反应少、收率高、分离提纯容易、操作费用低等显著的技术经济优势。

A kind of method for preparing the chloro- 3,3,3- trifluoroacetones of 1-

本发明公开了一种制备1‑氯‑3,3,3‑三氟丙酮的方法，以六氟‑2,3‑二氯‑2‑丁烯原料，先与乙醇钠的乙醇溶液反应，再经酸化和脱羧反应得到1‑氯‑3,3,3‑三氟丙酮。本发明提供的方法，具有原料易得、成本低、收率高、制备工艺温和、反应安全等优点。制备的1‑氯‑3,3,3‑三氟丙酮，适合用于合成医药、农药中间体和原料药。

Process for producing optically active 3,7-dimethyl-6-octenol and process for producing intermediate therefor

Cis-3,7-dimethyl-2,7-octadienylamine containing from 2 to 10% by weight cis-3,7-dimethyl-2,7-octadienylamine is prepared by subjecting a mixture of an alkylamine and isoprene in a molar ratio of 1:4 to 1:4.5 to telomerization at 80 to 100° C. for from 2.5 to 3.5 hours in the presence of an alkyllithium catalyst and/or phenyllithium catalyst.

Method for preparing natural benzaldehyde by spraying continuous hydrolysis

本发明公开了一种喷射连续水解制备天然苯甲醛的方法，属于农林化工产品的精深加工领域，一种喷射连续水解制备天然苯甲醛的方法包括以下步骤：S1：选取肉桂油或桂醛为原料，配制碱液作为水解液，S2：加热肉桂油或桂醛至60‑200°C，S3：将碱液注入水解釜的内部，加热碱液至沸腾并保持沸腾状态，S4：将加热至60‑200°C的肉桂油或桂醛以雾化方式喷入水解釜的内部，同时将沸腾状态的碱液以雾化方式重新喷入水解釜的内部，肉桂油或桂醛与碱液在水解釜的内部以喷射对冲的方式充分接触，水解产生苯甲醛。本发明的喷射连续水解制备天然苯甲醛的方法，采用加热的原料和沸腾的水解液以雾状形式喷射对冲的方式进行水解。

Method for producing 2'-trifluoromethyl group-substituted aromatic ketone

The present invention relates to a method for producing a 2'-trifluoromethyl group-substituted aromatic ketone, wherein a 2-halogen substituted benzotrifluoride compound is reacted with magnesium metal, and converts into a Grignard reagent, and the Grignard reagent is reacted with an acid anhydride, and then subjected to hydrolysis to produce a 2'-trifluoromethyl group-substituted aromatic ketone. The method for producing a 2'-trifluoromethyl group-substituted aromatic ketone of the present invention is capable of producing a 2'-trifluoromethyl group-substituted aromatic ketone without using costly raw materials, by generating a Grignard reagent as an intermediate, and effectively reacting the Grignard reagent with an acid anhydride. A 2'-trifluoromethyl group-substituted aromatic ketone produced by the method for producing a 2'-trifluoromethyl group-substituted aromatic ketone of the present invention can be used as a fine chemical, a pharmaceutical/agrochemical raw material, a resin/plastic raw material, an electronics/information material, an optical material or the like.

Production technique of difluoroacetone

本发明公开了一种二氟丙酮的生产工艺，采用间歇法工艺，分三步：1、二氟乙酸乙酯、乙酸乙酯和乙醇钠在温度－5℃－10℃反应生成二氟乙酰乙酸乙酯的钠盐，然后升温到20℃－50℃继续反应16－24小时，常压；2、将上述反应产物精馏分离出生成的乙醇，然后冷却到5℃－10℃调节pH=2，然后慢慢升温进行回流反应，再进行减压蒸馏得到中间产物二氟乙酰乙酸乙酯粗品3、将馏出产物：二氟乙酰乙酸乙酯粗品在酸催化下在20℃－100℃进行水解反应得到二氟丙酮粗品，提纯精馏操作，得到成品二氟丙酮。

Vinyl ether compounds and processes for preparing aldehyde compounds and a carboxylate compound therefrom

COMPUESTOS ETER-VINÍLICOS Y PROCESOS PARA PREPARARLOS. ETHER-VINYL COMPOUNDS AND PROCESSES TO PREPARE THEM.

Method of preparing 4-dichlorophenyl-1-tetralones

Method of preparing 4-disubstituted phenyl-1-tetralones of formula ##STR1## in which X represents halogen, C 1 -C 4 alkyl or C 1 -C 4 alkoxy and Y, situated in position 2' or 3', represents halogen or C 1 -C 4 alkyl, this method being characterized in that it comprises the reaction, in the presence of an acid agent, of α-naphthol of formula (II) with a phenyl compound of formula (III): ##STR2## where X represents halogen, C 1 -C 4 alkyl or C 1 -C 4 alkoxy, and Y is situated in the ortho or meta position with respect to X and represents halogen or C 1 -C 4 alkyl.

Carbonyl compound and process of preparing the same

1-methoxyl-2,6,10-trimethyl-1,3,5,9-undec-tetraene and preparation method and uses thereof

Procedimento per produrre tetraclorociclobutenone da esacloro ciclobutene

Preparation of 1-aryloxy-methyl ketones

1-(2,3,5,6-四氟苯基)-2,2-二甲基丙酮化合物及制备方法

一种1-(2,3,5,6-四氟苯基)-2,2-二甲基丙酮化合物，其结构式为：

一种1,2-环己二酮的制备方法

本发明属于化学合成技术领域，尤其涉及一种1,2‑环己二酮的制备方法。本发明提供的制备方法，将环已酮、盐酸和亚硝酸异戊酯混合进行成肟反应，得到成肟反应液后，调节所述成肟反应液的pH值≥7后，将pH值≥7的成肟反应液、水溶性亚硝酸盐和硫酸混合进行氧化水解反应，得到所述1,2‑环己二酮，所述盐酸的质量百分比≥35％，所述硫酸的质量百分比≤30％。本发明提供的制备方法无需进行除醇和过滤得到中间体，直接调节成肟反应液的pH值≥7，与水溶性亚硝酸盐和硫酸混合进行氧化水解反应得到目标产物1,2‑环己二酮，本发明采用一锅法成功制备1,2‑环己二酮，步骤简单，且1,2‑环己二酮产率高，适用工业生产。

环丁酮的合成新路线

本发明公开了一种合成环丁酮的新路线，将镁粉和溶剂混合，加入少量的碘和1,3‑二溴丙烷引发，在一定温度下，滴加1,3‑二溴丙烷和溶剂的混合液，得到格氏试剂；然后在一定温度下，滴加N‑甲氧基‑N‑甲基氨基甲酰氯和溶剂的混合液，保温2h，水解，酸化，干燥，蒸出溶剂得到含量99%以上的纯品，收率50%以上。该合成路线条件温和，副产少，原料易得价廉，环境友好，较适合于较大规模工业化生产。

一种1,2-环己二酮的制备方法

本发明属于化学合成技术领域，尤其涉及一种1,2‑环己二酮的制备方法。本发明提供的制备方法，将环已酮、盐酸和亚硝酸异戊酯混合进行成肟反应，得到成肟反应液后，调节所述成肟反应液的pH值≥7后，将pH值≥7的成肟反应液、水溶性亚硝酸盐和硫酸混合进行氧化水解反应，得到所述1,2‑环己二酮，所述盐酸的质量百分比≥35％，所述硫酸的质量百分比≤30％。本发明提供的制备方法无需进行除醇和过滤得到中间体，直接调节成肟反应液的pH值≥7，与水溶性亚硝酸盐和硫酸混合进行氧化水解反应得到目标产物1,2‑环己二酮，本发明采用一锅法成功制备1,2‑环己二酮，步骤简单，且1,2‑环己二酮产率高，适用工业生产。