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40 results about "Methyl malonate" patented technology

Dimethyl malonate is a diester derivative of malonic acid. It is a common reagent for organic synthesis used, for example, as a precursor for barbituric acid. It is also used in the malonic ester synthesis.

Process method for preparing fluopyram key intermediate

The invention discloses a process method for preparing a fluopyram key intermediate. The key intermediate is [3-chloro-5-(trifluoromethyl) pyridine-2-yl] ({[2-(trifluoromethyl) benzoyl] amino} methyl) dimethyl malonate, and the process method comprises the following steps: in the presence of a solvent 1, carrying out a reaction on a compound 2-[3-chloro-5-(trifluoromethyl) pyridyl] dimethyl malonate potassium salt and a compound 1-D in a reaction container, and distilling and recovering the solvent 1 to obtain the intermediate compound. Wherein the solvent 1 is selected from acetic ester solvents with the boiling point range of 40-110 DEG C at normal temperature and normal pressure. The process method is simple and convenient, the total yield is high, the solvent is easy to recover, and the product purity is high; the intermediate does not need purification post-treatment, can be directly used for synthesis of fluopyram, can be amplified, and is beneficial to cost reduction, efficiency improvement and commercial mass production.
Owner:YIFAN BIOTECHNOLOGY (SHANGHAI) CO LTD

Process method for preparing fluopyram

The invention discloses a process method for preparing fluopyram. The process method comprises the following steps: in the presence of a solvent 1, reacting a compound 2-[3-chloro-5-(trifluoromethyl) pyridyl] dimethyl malonate potassium salt with a compound 1-D in a reaction container to obtain an intermediate compound, and distilling to recover the solvent 1 without purification treatment of the intermediate compound; adding water, alkali and a solvent 2 into the reaction container for reaction; adjusting the pH value after the reaction, and continuing the reaction; and after the reaction is finished, carrying out post-treatment to obtain the product fluopyram. Wherein the solvent 1 is selected from acetic ester solvents with the boiling point range of 40-110 DEG C at normal temperature and normal pressure. The process method is simple, convenient, high in total yield, low in cost and stable and qualified in product quality, fluopyram is prepared through a one-pot method, production equipment is reduced, investment is reduced, cost is reduced, efficiency is improved, and commercialized mass production is facilitated.
Owner:YIFAN BIOTECHNOLOGY (SHANGHAI) CO LTD

Pimobendan intermediate and synthesis method thereof

ActiveCN119431250Ashort route stepseasy to operateOrganic chemistryNitrationAcyl group
The present invention discloses a pimobendan intermediate synthesis method, which comprises: 1, carrying out a Friedel-Crafts acylation reaction on a compound I and a compound A in an aprotic solvent under the effect of a Lewis acid to generate a compound II; 2, ether is used as a solvent, under the alkaline condition, the compound II and dimethyl malonate or diethyl malonate are subjected to a substitution reaction, the generated compound is subjected to a hydrolysis reaction in an aqueous alkali solution, and a compound III is generated; and 3, heating the compound III under the conditions of hydrazine hydrate and acid to generate a compound IV, namely the pimobendan intermediate. The synthesis method cancels a nitration reaction step which is high in risk and generates a large amount of waste acid water, and is short in route step and simple to operate.
Owner:LIAONING FUYIN BIOTECHNOLOGY CO LTD

Post-treatment method for preparing dipropylmalonic acid crude product by dimethyl malonate method

The invention belongs to the technical field of separation of drug intermediates, and particularly relates to a method for preparing a high-purity dipropylmalonic acid refined product by adding a polar solvent into a dipropylmalonic acid crude product, heating, pulping for a certain time, cooling, filtering and drying. Decarboxylating the refined dipropylmalonic acid product to obtain high-purity valproic acid; distilling the filtrate to recover the polar solvent to obtain 2-methyl-2-propylmalonic acid, and carrying out decarboxylation on the 2-methyl-2-propylmalonic acid to obtain 2-methylpentanoic acid; 2-methylvaleric acid is used as a perfume additive. According to the method disclosed by the invention, the process impurity 2-methyl-2-propylmalonic acid in dipropylmalonic acid is separated, and the process impurity 2-methylvaleric acid (EP-L) in valproic acid or sodium valproate is precisely separated; the quality of the valproic acid product prepared by the method disclosed by the invention meets the requirements of European Pharmacopoeia EP-11 (2023). According to the invention, the problems of quality control and process evaluation of valproic acid or sodium valproate prepared by a dimethyl malonate method are solved.
Owner:HUNAN UNIV

Synthesis method of 5-bromoindole-2-carboxylic acid methyl ester

The invention discloses a synthesis method of 5-bromoindole-2-carboxylic acid methyl ester, and the synthesis route comprises the following steps: S1, taking 2-iodo-4-broronitrobenzene and dimethyl malonate as raw materials, and under the catalysis of a solid sulfonic acid resin catalyst, carrying out nucleophilic substitution reaction to prepare 2-(5-bromo-2-nitrophenyl) dimethyl malonate; s2, taking the dimethyl 2-(5-bromo-2-nitrophenyl) malonate prepared in the step S1 as a raw material, taking a ZSM-5 molecular sieve loaded with cobalt acetate as a catalyst, and introducing hydrogen for reduction reaction to prepare a 5-bromoindole-2-carboxylic acid methyl ester crude product; and S3, carrying out recrystallization on the 5-bromoindole-2-carboxylic acid methyl ester crude product prepared in the step S3 by using ethanol, so as to prepare a 5-bromoindole-2-carboxylic acid methyl ester pure product. The synthesis yield is relatively high, the environmental protection property is relatively good, and the prepared 5-bromoindole-2-carboxylic acid methyl ester is relatively excellent in quality and relatively low in cost.
Owner:ZHEJIANG JIANGBEI PHARMA

Method for detecting dipropylmalonic acid and impurities thereof

PendingCN121186232AComponent separationPharmaceutical SubstancesMonomethyl malonate
The invention belongs to the technical field of medicine detection, and particularly relates to dipropyl malonic acid prepared by a dimethyl malonate method and a detection method of impurities of the dipropyl malonic acid. According to the detection method provided by the invention, the dipropyl malonic acid prepared by a dimethyl malonate method and impurities thereof are detected through high performance liquid chromatography (HPLC) for the first time; the impurities comprise propyl malonic acid, 2-methyl-2-propyl malonic acid, 2-propyl-2-butyl malonic acid, propyl malonic acid monomethyl ester, 2-methyl-2-propyl malonic acid monomethyl ester, dipropyl malonic acid monomethyl ester, 2-propyl-2-butyl malonic acid monomethyl ester, propyl malonic acid dimethyl ester, dipropyl malonic acid monopropyl ester and propyl malonic acid dimethyl ester; the invention relates to a method for preparing dipropyl malonic acid, which is selected from one or more of dipropyl malonic acid dimethyl ester, dipropyl malonic acid methyl ester propyl ester and 2-propyl-2-butyl malonic acid dimethyl ester, and solves the problems of quality control and process evaluation of dipropyl malonic acid serving as an intermediate of sodium valproate prepared by a dimethyl malonate method.
Owner:HUNAN XIANGZHONG PHARM CO LTD

Gram-level synthesis method of Dactyllactone A

The invention discloses a gram-level synthesis method of Dactyllactone A. The gram-level synthesis method of Dactyllactone A is shown in the description. The method comprises the following steps: with simple and easily available aryl iodide, aziridine and triisopropyl silylacetylene as starting materials, stirring and reacting in an organic solvent at 60-70 DEG C under the action of a palladium catalyst, a phosphine ligand, a norbornene derivative and alkali to obtain a key intermediate; the key intermediate is condensed with iodo gem-dimethyl ester furanone prepared from propiolic acid and dimethyl malonate iodine ylide, and then the condensation product is subjected to an Au / Ag catalyzed intramolecular hydroamination reaction, photocatalytic 6-pi electro-cyclization and two-step conversion, so that the natural product Dactyllactone A can be obtained, wherein the iodo gem-dimethyl ester furanone and iodo gem-dimethyl ester furanone are prepared from propiolic acid and dimethyl malonate iodine ylide. The method has the advantages of cheap and easily available raw materials, short reaction steps, high reaction efficiency, large preparation scale, simple preparation process and the like, has great application potential, and lays a good foundation for industrial production.
Owner:WUHAN UNIV

A process for the preparation of a key intermediate for iodopyrimidines

PendingCN122277514AHydrolysisHydroxylation
This invention discloses a method for preparing a key intermediate of iodopyridine, using dimethyl malonate as a raw material, and sequentially undergoing dihydroxylation S1 → acetalization S2 → hydrolysis and acidification S3 → decarboxylation S4 to obtain iodopyridine. The raw materials of this invention are inexpensive and readily available in the market, and the reaction efficiency is high, improving the purity and yield of the product. Intermediates 1 and 2 obtained from the process do not require separation and purification operations and can be directly used in the next step of the reaction. The purification effect is significant, yielding intermediate products with a purity ≥99%, and the total yield of the five steps is as high as 65-70%, which is beneficial for large-scale production.
Owner:JIANGSU YUTIAN PHARM CO LTD

Preparation method of pinoxaden

The invention discloses a preparation method of pinoxaden, and belongs to the field of organic synthesis. The synthesis method comprises the following synthesis steps: (1) reacting dimethyl malonate with hydrazine hydrate under the action of alkali to generate pyrazolidine-3, 5-diketone; (2) carrying out cyclization on the pyrazolidine-3, 5-diketone and diethylene glycol dimethanesulfonate to generate dihydro-1H-pyrazolo [1, 2-d] [1, 4, 5] oxadiaze-7, 9 (2H, 8H)-diketone; (3) carrying out a coupling reaction on the dihydro-1H-pyrazolo [1, 2-d] [1, 4, 5] oxadiaze-7, 9 (2H, 8H)-diketone and 2, 6-diethyl-4-methyl bromobenzene, so as to obtain 8-(2, 6-diethyl-4-methyl phenyl)-tetrahydropyrazolo [1, 2-d] [1, 4, 5] oxadiaze-7, 9-diketone; and (4) carrying out a reaction on the 8-(2, 6-diethyl-4-methylphenyl)-tetrahydropyrazolo [1, 2-d] [1, 4, 5] oxadiaza-7, 9-diketone and pivaloyl chloride to generate the pinoxaden. The method disclosed by the invention is simple to operate, mild in reaction condition and suitable for industrial mass production.
Owner:BENGBU COLLEGE

A method for preparing an antiepileptic drug, magnesium valproate

The present application relates to the preparation method of magnesium valproate shown in chemical structural formula I: under the action of potassium carbonate and PTC, dimethyl malonate is subjected to dipropylization with 1-chloropropane in DMF solvent to prepare dimethyl dipropyl malonate shown in formula III; III is subjected to hydrolysis reaction to prepare dipropyl malonic acid shown in formula II; II is uniformly mixed with magnesium oxide, and heated to prepare magnesium valproate shown in formula I by decarboxylation, and the total yield of magnesium valproate is not less than 90.0%; the preparation reaction is as follows: wherein, the PTC for dipropylization is selected from quaternary ammonium salt, the reaction temperature is 50-140 DEG C, the reaction time is 4.0-14.0 h; the hydrolysis temperature is 70-95 DEG C, the time is 2.0-4.0 h; the decarboxylation temperature is 140-158 DEG C, and the time is 3.0-5.0 h.
Owner:HUNAN UNIV

A method for the synthesis of pimobendan

The application discloses a synthesis method of pimobendan, which comprises the following steps: a Friedel-Crafts acylation reaction: compound I and compound A are subjected to a Friedel-Crafts acylation reaction in aprotic solvent under the action of a Lewis acid to generate compound II; a substitution and hydrolysis reaction: under alkaline conditions, compound II and dimethyl malonate or diethyl malonate are subjected to a substitution reaction in an ether solvent, and the generated compound is subjected to a hydrolysis reaction in an alkaline aqueous solution to generate compound III; a decarboxylation and ring-closing reaction: compound III is heated under the condition of hydrazine hydrate and acid to generate compound IV; a substitution reaction: compound IV and an amine are subjected to a substitution reaction in a polar solvent to generate compound V; a reduction reaction: compound V is subjected to a reaction in an acidic aqueous solution of a protic solvent under the condition of palladium-carbon and hydrogen to generate compound VI; and a ring-closing reaction, so that the pimobendan is obtained. The method has high safety, short line steps and simple operation.
Owner:LIAONING FUYIN BIOTECHNOLOGY CO LTD

A method for synthesizing 2-chloro-6-nitrotoluene

The present invention relates to the field of organic synthesis, and particularly relates to a new method for synthesizing 2-chloro-6-nitrotoluene. The synthesis method of 2-chloro-6-nitrotoluene provided by the present invention uses 2,3-dichloronitrobenzene (Compound 1) as a raw material, reacts with methyl cyanoacetate or dimethyl malonate under the action of a reaction solvent and an acid-binding agent to form Compound 2, and after filtration and decolorization, a dilute acid solution is added for de-esterification reaction to obtain Compound 3. Finally, the R group is removed in a dilute acid solution to obtain the final product 2-chloro-6-nitrotoluene (Compound 4). The synthesis method of 2-chloro-6-nitrotoluene described in the present invention has the advantages of simple operation, safety, economy, environmental friendliness, and low cost.
Owner:PAPANNA (BEIJING) TECH CO LTD

Method for synthesizing sex pheromone of pinus tabulaeformis

The invention relates to the field of biopesticides, in particular to a method for synthesizing sex pheromone of pinus tabulaeformis, which comprises the following steps: reacting 1-bromo-n-heptane (3) serving as an initial raw material with magnesium, and then reacting with (R)-epoxypropane (4) to obtain chiral alcohol 5; then reacting with paratoluensulfonyl chloride, and then reacting with dimethyl malonate to obtain malonate 7; carrying out sodium hydroxide catalytic hydrolysis and high-temperature decarboxylation to obtain an acid 8, and carrying out lithium aluminum hydride reduction and NBS bromination to obtain a chiral bromide 10; reacting with magnesium, and reacting with sulfonate 12 to obtain silyl ether 11; then carrying out TBAF deprotection to obtain chiral alcohol 13; and finally, reacting the chiral alcohol 13 with acetic acid to obtain acetic acid (2S, 3S, 7S)-3, 7-dimethyl-2-pentadecanol ester (1), and reacting the chiral alcohol 13 with propionic acid to obtain propionic acid (2S, 3S, 7S)-3, 7-dimethyl-2-pentadecanol ester (2). The method has the advantages of high total yield, low synthesis cost and the like.
Owner:CHINA AGRI UNIV

Environment-friendly gasoline antiknock agent and preparation method thereof

The present application belongs to the field of gasoline additive, and particularly relates to an environment-friendly gasoline antiknock agent and a preparation method thereof. The antiknock agent comprises two newly designed modified compounds: 3,5-di-tert-butyl phenyl carborane carboxylate and 2-(dicyclohexyl phosphino)-1,2-oxaborinin-4-carboxylic acid iso-octyl ester. In the preparation, a cosolvent is first added into a reactor, and then the two modified compounds, polyisobutylene amine, isobutyl acetate and dimethyl malonate are sequentially added under an inert atmosphere. After mixing by continuous stirring, the temperature is raised, an antioxidant is added, and then stirring is continued. Finally, the product is obtained by cooling and filtering. The two modified compounds are prepared by condensation reaction of carborane carboxylic acid and steric phenol, esterification of oxaborinin carboxylic acid and iso-octanol, and then phosphination reaction. The antiknock agent does not contain metal elements, has biodegradable characteristics, can significantly improve the octane number of gasoline and reduce engine deposits and harmful gas emissions, and meets the green environmental protection requirements.
Owner:SHANDONG DONGCHANG FINE CHEM TECH CO LTD

Method for synthesizing dimethyl malonate through homogeneous-phase continuous carbonylation

The invention discloses a method for synthesizing dimethyl malonate through homogeneous-phase continuous carbonylation, which comprises the following steps of: carrying out carbonylation reaction on chloracetate serving as a raw material at a certain temperature and pressure in the presence of a liquid acid-binding agent and a catalyst to synthesize the dimethyl malonate. The problems that in a batch process of a traditional dimethyl malonate carbonylation synthesis method, carbon monoxide in a reactor is high in pressure and large in consumption, and once leakage or other faults occur, great risks are brought to safety production are solved; the invention solves the technical problems in the prior art that an acid-binding agent is in a solid state before and after acid-binding, the solid content is high, if continuous production transformation is needed, the requirement for feeding and discharging conveying of equipment is high, large-scale production is not facilitated, and the product and a catalyst are difficult to separate and recover after the reaction is finished, so that the production cost is increased.
Owner:ANSHAN HIFICHEM CO LTD

Synthesis method of methyl cis-dihydrojasmonate

The invention belongs to the technical field of spice raw material synthesis, and particularly relates to a synthesis method of methyl cis-dihydrojasmonate, which comprises the following steps: dissolving 1-heptyne in toluene, discharging into a first reaction tank, adding a cobalt catalyst, and discharging 1-bromine-ethylene and carbon monoxide gas into the first reaction tank; adding triphenylphosphine into a first catalyst recovery tank, discharging catalyst precipitates, and carrying out sectional distillation to distill, cool and recover 1-heptyne; absolute methanol is discharged into the layering tank; dimethyl malonate is discharged into a second reaction tank, sodium methoxide is slowly added, an addition reaction is carried out at the temperature of-5 DEG C to 0 DEG C, and then heating is carried out for a decarboxylation reaction; 4-bromo-dihydrojasmonic acid methyl ester obtained by distillation is discharged into a third reaction tank; and discharging methyl jasmonate with alpha, beta-double bonds into a fourth reaction tank for reaction. By simplifying the steps, improving the recovery rate of the catalyst and realizing continuous production, the problems of high cost, low yield, low recovery rate of the catalyst and the like in preparation of the methyl cis-dihydrojasmonate in the prior art are solved.
Owner:TENGZHOU XINHE BIOTECHNOLOGY CO LTD

A method for efficiently synthesizing a puquimafine intermediate

This invention discloses a highly efficient method for synthesizing proxalutamide intermediates, belonging to the field of pharmaceutical synthesis technology. First, dimethyl malonate and 2-chloro-5-nitropyridine are used as raw materials, condensed in the presence of potassium carbonate to generate dimethyl 2-(5-nitropyridine-2-yl)malonate. This is then reacted with tert-butyl acrylate and acid-hydrolyzed to obtain 4-(5-nitropyridine-2-yl)butyric acid. After activation with N,N'-carbonyl diimidazole, it is coupled with aminoacetaldehyde dimethyl acetal to form N-(2,2-dimethoxyethyl)-4-(5-nitropyridine-2-yl)butyramide. Then, a cyclization reaction mediated by phosphorus pentoxide and methanesulfonic acid is used to generate crude 2-(3-(5-nitropyridine-2-yl)propyl)oxazole. After purification, the nitro group is reduced by catalytic hydrogenation, and finally, it reacts with 1,5-naphthalenedisulfonic acid to form a salt, yielding the proxalutamide intermediate. This method achieves highly efficient synthesis of proxalutamide intermediates.
Owner:ANHUI MENOVO PHARM CO LTD

Synthesis method of pimobendan

ActiveCN119431326Ashort route stepseasy to operateOrganic chemistryAcyl groupHydrolysis
The invention discloses a synthesis method of pimobendan, which comprises the following steps: Friedel-Crafts acylation reaction: carrying out Friedel-Crafts acylation reaction on a compound I and a compound A in an aprotic solvent under the action of Lewis acid to generate a compound II; substitution and hydrolysis reaction: ether is used as a solvent, under the alkaline condition, the compound II and dimethyl malonate or diethyl malonate are subjected to substitution reaction, the generated compound is subjected to hydrolysis reaction in aqueous alkali, and a compound III is generated; decarboxylation ring closing reaction: heating the compound III under the conditions of hydrazine hydrate and acid to generate a compound IV; substitution reaction: carrying out substitution reaction on the compound IV and amine in a polar solvent to generate a compound V; reduction reaction: reacting the compound V in an acidic aqueous solution of a protonic solvent under the conditions of palladium carbon and hydrogen to generate a compound VI; and carrying out ring closing reaction to obtain the pimobendan. The method is high in safety, short in circuit step and simple to operate.
Owner:LIAONING FUYIN BIOTECHNOLOGY CO LTD

A process for the preparation of fluopyram

The application discloses a preparation method of fluopyram, which comprises the following steps: step 1: in the presence of solvent 1 and a base, dimethyl malonate and 2,3-dichloro-5-trifluoromethyl pyridine are added to react, a salt reaction is carried out by adjusting pH, and 2-[3-chloro-5-(trifluoromethyl) pyridyl] dimethyl malonate potassium salt, namely intermediate 1, is obtained; step 2: o-trifluoromethyl benzoyl chloride, an organic base and chloromethylamine are added to react, and intermediate 2 is obtained; step 3: solvent 3, intermediate 1 and intermediate 2 are added to react, and intermediate 3 is obtained; step 4: water, a base, solvent 4 and intermediate 3 are added, pH is adjusted after reaction, and continuous reaction is carried out, and fluopyram is obtained. By adopting the preparation method, the yield of fluopyram is high, the purity is high, the reaction time is short, the reaction condition is mild, and the method is suitable for mass production.
Owner:YIFAN BIOTECHNOLOGY (SHANGHAI) CO LTD

Near-infrared photocatalytic coupling method of 2-benzene-1,2,3,4-tetrahydroisoquinoline compounds with nucleophiles

This invention discloses a near-infrared photocatalytic coupling method for 2-benzene-1,2,3,4-tetrahydroisoquinoline compounds with nucleophiles. The method uses (MV)Bi₂I₈ type perovskite as a catalyst, wherein the organic portion of the catalyst, MV… 2+ The product is a methyl viologen cation. 2-Benzene-1,2,3,4-tetrahydroisoquinoline compounds are reacted with nucleophiles (dimethyl malonate, nitromethane, ethyl nitrosyl acetate) under light irradiation at room temperature or in air to undergo cross-dehydrogenation coupling reactions to obtain the corresponding product. This invention is simple to operate, operates under mild conditions, and uses readily available catalysts. It successfully achieves cross-dehydrogenation coupling between substrates using only near-infrared light, and yields high product yields.
Owner:SHAANXI NORMAL UNIV

Pyrazole herbicide intermediate and its preparation method

The present invention relates to an intermediate of a pyrazole herbicide and a preparation method thereof. Compound (1) reacts with dimethyl malonate to synthesize compound (2), and compound (2) undergoes cyclization under alkaline conditions to synthesize compound (3). The present invention provides a simple, safe, environmentally friendly, high-conversion-rate and low-cost synthesis method.
Owner:PAPANNA (BEIJING) TECH CO LTD

Preparation method of naphthylacetic acid

The invention discloses a preparation method of naphthylacetic acid, which comprises the following steps: reacting a compound (halogenated naphthalene) in a formula I with diethyl malonate or dimethyl malonate to obtain a compound in a formula II, performing ester hydrolysis on the compound in the formula II to obtain a compound in a formula III, and performing decarboxylation reaction to obtain a compound naphthylacetic acid in a formula IV. The process for synthesizing naphthylacetic acid is low in cost, simple and convenient to operate, good in yield, environment-friendly and suitable for industrial production. # imgabs0 #
Owner:HANGZHOU LEDUN TECH CO LTD

Recovery and utilization of 2-methyl-2-propylmalonic acid

The invention belongs to the technical field of separation of drug intermediates, and particularly relates to recovery and application of 2-methyl-2-propylmalonic acid. The method comprises the following steps: adding a polar solvent into a dipropylmalonic acid crude product prepared by a dimethyl malonate method, heating, pulping for a certain time, cooling, filtering and drying to obtain high-purity dipropylmalonic acid; and distilling the filtrate to recover the polar solvent to obtain the 2-methyl-2-propylmalonic acid as shown in the formula I. The HPLC (High Performance Liquid Chromatography) of the 2-methyl-2-propylmalonic acid is greater than 99.0% (Figure 1). The 2-methyl-2-propylmalonic acid is an intermediate for preparing the spices, namely the 2-methylpentanoic acid; and carrying out decarboxylation on the 2-methyl-2-propyl malonic acid to obtain the 2-methylvaleric acid.
Owner:HUNAN XIANGZHONG PHARM CO LTD +1

A method for synthesizing high purity δ-lactones

The present application relates to the technical field of delta-lactone synthesis, in particular to a high-purity delta-lactone synthesis method, comprising the following steps: using potassium carbonate to catalyze Michael addition reaction of the active methylene functional group of dimethyl malonate and the alpha, beta-alkenyl functional group of 1-octene-3-ketone to generate intermediate product I; intermediate product I generates decarboxylation reaction under the catalysis of boric acid to generate intermediate product II; chiral ligand supported nickel catalyst catalyzes asymmetric hydrogenation reaction of the delta-carbonyl functional group of intermediate product II to generate chiral delta-hydroxyl functional group, and ester exchange reaction of the chiral delta-hydroxyl functional group and the ester functional group of intermediate product II to generate chiral delta-decalactone. The present application designs and synthesizes four chiral ligand supported nickel catalysts on one hand, and designs a new route capable of synthesizing chiral delta-decalactone with high optical purity on the other hand.
Owner:JIANGXI XIANGHAI BIOLOGICAL TECH CO LTD

A novel method for producing N,N'-bis[2-(1H-imidazol-4-yl)ethyl]malonamide

A process for producing N,N'-bis[2-(1H-imidazole-4-yl)ethyl]malonamide of formula (I) by reacting dimethyl malonate with histamine in a polar organic solvent at a temperature of 85°C to 120°C, the process comprising a step of crystallization from water and / or a polar organic solvent. The process makes it possible to produce a product with a purity of 99.0% by weight and suitable for the production of substances in the pharmaceutical industry.
Owner:OBSHCHESTVO S OGRANICHENNOJ OTVETABTVENNOSTJU VALENTA INTELLEKT +1

A method for synthesizing an enoxamide intermediate, 5-[2-(ethylthio)propyl]-3-hydroxy-2-cyclohexen-1-one

The present application belongs to the field of chemical synthesis and pesticides, and particularly relates to a preparation method of an enoxacin intermediate 5-[2-(ethylthio)propyl]-3-hydroxy-2-cyclohexen-1-ketone. The present application comprises: using 3-ethylthiobutyraldehyde and methyl acetoacetate as raw materials, generating 2-acetyl-5-(ethylthio)hex-2-enate acid methyl ester through a Brain-Von Eggers reaction, then performing Michael addition and Claisen ester condensation with dimethyl malonate, and then performing hydrolysis through sodium hydroxide, and heating decarboxylation through hydrochloric acid to obtain 5-[2-(ethylthio)propyl]-3-hydroxy-2-cyclohexen-1-ketone. The preparation method is simple, convenient to operate, and easy to be scaled up in industry, and finally, the total yield of the similar one-pot reaction is as high as 77%.
Owner:ZHEJIANG UNIV OF TECH +1

Modified poly (butylene terephthalate)-co-adipate and preparation method thereof

The invention relates to the technical field of biodegradable polyester, and provides modified poly (butylene terephthalate)-co-adipate and a preparation method thereof. The repetitive structure unit of the modified poly (terephthalic acid-co-butylene adipate) comprises a terephthalic acid structure unit, an adipic acid structure unit, a 1, 4-butylene glycol structure unit and a fourth monomer structure unit; the fourth monomer comprises at least one of oxalic acid, dimethyl oxalate, furandicarboxylic acid, dimethyl furandicarboxylate, malonic acid, dimethyl malonate, methylmalonic acid and diethyl methylmalonate. Compared with conventional pure PBAT, the modified poly (butylene terephthalate-co-butylene adipate) provided by the invention has higher glass transition temperature and breaking strength, lower melt index and better product hue, and can meet the use requirements of PBAT; and various problems caused by poor heat resistance and strength in the processing process and subsequent application of the conventional PBAT product are effectively solved.
Owner:CHINA PETROLEUM & CHEMICAL CORP

Preparation method of clethodim intermediate

The invention relates to a preparation method of a clethodim intermediate, which comprises the following steps: carrying out addition reaction on dimethyl malonate and 6-ethylthio-3-heptene-2-ketone in the presence of a catalytic amount of dimethyl malonate sodium salt to generate an intermediate compound shown as a formula (3), # imgabs0 #
Owner:HEBEI LANSHENG BIOTECH CO LTD +1

Synthesis method of methyl cyclopentyl formate

The invention provides a synthetic method of methyl cyclopentyl formate, and relates to the technical field of synthesis of organic chemical intermediates. The synthesis of the cyclopentyl methyl formate comprises the following steps: carrying out substitution cyclization reaction on 1, 4-dihalogenated butane serving as an initial raw material and dimethyl malonate to obtain 1, 1-cyclopentyl dimethyl dicarboxylate, and carrying out Krapcho degreasing reaction on the 1, 1-cyclopentyl dimethyl dicarboxylate to obtain a target compound, namely the cyclopentyl methyl formate. The method overcomes the defects in the prior art, is simple in synthesis route, low in raw material cost and easy to obtain, is suitable for industrial production, and provides a new synthesis scheme for synthesis and preparation of methyl cyclopentyl formate.
Owner:CHENGDA PHARM CO LTD

Preparation method of antiepileptic drug magnesium valproate

The invention relates to a preparation method of magnesium valproate as shown in a chemical structural formula I. The preparation method comprises the following steps: carrying out dipropylation on dimethyl malonate and 1-chloropropane in a DMF (Dimethyl Formalonate) solvent under the action of potassium carbonate and PTC (Positive Temperature Coefficient) to prepare dimethyl dipropyl malonate as shown in a formula III; carrying out hydrolysis reaction on the dipropyl malonic acid III to prepare dipropyl malonic acid as shown in a formula II; uniformly mixing II with magnesium oxide, heating and decarboxylating to prepare magnesium valproate as shown in the formula I, wherein the total yield of magnesium valproate is not less than 90.0%; the preparation reaction is as follows: # imgabs0 #, the PTC of dipropylation is selected from quaternary ammonium salt, the reaction temperature is 50-140 DEG C, and the reaction time is 4.0-14.0 h; the hydrolysis temperature is 70-95 DEG C, and the hydrolysis time is 2.0-4.0 h; the decarboxylation temperature is 140-158 DEG C, and the decarboxylation time is 3.0-5.0 hours.
Owner:HUNAN UNIV