38results about "Preparation from nitriles" patented technology

The invention belongs to the technical field of fine chemical engineering, and discloses a synthesis method of a malonate compound, which comprises the following steps: under the action of a heterogeneous catalyst, carrying out hydrolysis-esterification reaction on cyanoacetic acid and alcohol, and after the reaction is finished, carrying out post-treatment to obtain the malonate compound, the heterogeneous catalyst comprises a carrier and an active component; the active component comprises ionic liquid and active metal; the carrier is an ordered mesoporous material; the active metal is alkaline earth metal. According to the method, malonate products can be obtained, the problems of low yield, serious equipment corrosion and large amount of three wastes are solved, efficient synthesis of malonate compounds is realized, meanwhile, the production efficiency is improved, and the environmental pollution is greatly reduced.

The invention provides a preparation method of hexafluoroisobutene, which comprises the following steps: firstly, reacting hexafluoroisopropanol with p-toluenesulfonyl chloride to generate an organic phase, then reacting with a cyano source to obtain 3, 3, 3-trifluoro-2-(trifluoromethyl) propionitrile, then reacting with an acid solution and a reducing agent in sequence to obtain hexafluoroisobutanol, and finally reacting with an acid solution and a reducing agent to obtain the hexafluoroisobutanol. And finally, carrying out alkali dehydration to generate hexafluoroisobutene. The preparation method provided by the invention is simple in process route and mild in reaction condition, the solvent used in the preparation process can be recycled, the pollution in the preparation process is reduced, and the preparation method is less in three wastes, environment-friendly and suitable for large-scale production.

The invention relates to the technical field of high-temperature-resistant low-dielectric polymer materials, in particular to a compound containing an adamantane structure, a preparation method of the compound, polyimide and a preparation method of the polyimide, and the compound containing the adamantane structure has at least one of the following structures shown in the specification, in the formula (I), R1 and R2 independently represent-H, a C1-6 alkyl group, a halogenated C1-6 alkyl group, a methoxy group, a phenyl group, a trifluoromethyl group,-F,-Cl or-Br. The compound containing the adamantane structure provided by the invention has high symmetry and can be used as a raw material for preparing polyimide, so that the prepared polyimide is low in dielectric constant and excellent in optical performance.

The application provides a method for preparing carboxylic acid by hydrolysis of nitrile, wherein the nitrile and protonic acid are subjected to hydrolysis reaction in a microwave reactor in the presence of solid inorganic medium to obtain the carboxylic acid; wherein the frequency of the microwave reactor is 0.9-3.0 GHz; the nitrile is aliphatic nitrile, aromatic nitrile or a mixture thereof; the relative dielectric constant ε of the solid inorganic medium is 30-500. r The application realizes microwave-high dielectric medium coupling reinforcement through the cooperation of the solid inorganic medium with specific relative dielectric constant and specific microwave reaction condition, can realize the efficient obtaining of high-purity carboxylic acid product, and produces ammonium salt as by-product. The overall method has high yield, strong raw material universality, is easy to be industrialized and amplified, and has remarkable economic effect.

The invention discloses a preparation method of 2, 6-dialkoxy or sulfenyl benzoic acid, and the synthesis route of the method is as follows: X1, X2, Y, R1 and R2 are defined in the specification. Compared with the existing process route, the preparation method disclosed by the invention has the characteristics of mild reaction conditions, simplicity in operation, low production cost, easiness in industrialization and the like.

The present disclosure provides techniques for assessing FADS1 activity in a patient. Also provided are techniques for determining the appropriateness of treating a patient with a FADS1-modulating (e.g., inhibiting) compound. This determination can be made by analyzing one or more biological indicators of a FADS1-mediated disease or disorder in the subject. The one or more biological indicators can include one or more of the following in the subject: ratios of polyunsaturated fatty acids ("PUFAs"), the relative abundance of one or more cell types, the relative abundance of one or more differentially expressed genes ("DEGs") (or gene signatures of such DEGs, e.g., RNA), and / or the relative abundance of one or more metabolites. Also disclosed are methods of using FADS1 inhibitors in methods for treating metabolic disorders and obesity.

The application belongs to the technical field of pharmaceutical chemistry synthesis, and particularly relates to a synthesis method of a fluorofelarana intermediate 2-methyl-4-acetylbenzoic acid. In the application, o-chlorotoluene and acetyl chloride are reacted under the action of anhydrous aluminum chloride to generate 4-chloro-3-methylacetophenone; the 4-chloro-3-methylacetophenone and acetonitrile are catalyzed by Ni to generate 4-acetyl-2-methylbenzonitrile; and then the 4-acetyl-2-methylbenzonitrile is hydrolyzed to generate 2-methyl-4-acetylbenzoic acid. The application has the beneficial effect that acetonitrile is used as a cyanogen to replace halogen, and a highly toxic cyanide is abandoned, so that the whole process is safer and more environmentally friendly, the production of three wastes is reduced, and the synthesis cost of 2-methyl-4-acetylbenzoic acid is greatly reduced.

The invention relates to a treprostinil monohydrate crystal and a preparation method thereof. The present invention provides novel crystalline forms of treprostinil monohydrate, mixtures comprising the same, and methods of making the same.

The present invention, as disclosed herein, relates to compounds, combinations, kits, and methods of using them for use in bioorthogonal release reactions. In particular, the compounds, combinations, and kits of the present invention can be used to achieve rapid and efficient click release. The applications of the compounds, combinations, and kits of the present invention include both in vitro and in vivo applications.

This invention provides a composite catalyst for the hydrolysis of cyanoacetic acid and a method for synthesizing malonic acid ester. This invention belongs to the field of fine chemical technology. The composite catalyst includes an active component, a modifier, and a support. The active component includes a main active component and an auxiliary component. The main active component contains Fe. 3+ The additive component comprises ruthenium, copper, cobalt, and cerium metal ions, and the modifier is a sulfosuccinate surfactant. This invention solves the problem of side reactions caused by the use of strong acid catalysts during the hydrolysis of cyanoacetic acid in the prior art. It also solves the problems of low product yield and large amounts of waste, achieving efficient synthesis of malonic acid and malonic esters while reducing production costs and environmental pollution, thus facilitating the large-scale industrial production of malonic acid esters.

The invention belongs to the technical field of organic synthetic chemistry, and particularly relates to a fluorine-containing hydroxybenzoic acid compound and a preparation method thereof. The invention provides a brand-new synthesis route and method, which comprises the following steps: by taking 4-fluoro-3-methoxybenzonitrile as an initial raw material, firstly, carrying out specific demethylation reaction in a benzene or toluene solvent under the catalysis of anhydrous aluminum trichloride to obtain an intermediate 4-fluoro-3-hydroxybenzonitrile; then carrying out acidic hydrolysis reaction on the intermediate in a mixed medium of concentrated sulfuric acid and water to convert cyano into carboxyl to obtain a 3-hydroxy-4-fluorobenzoic acid crude product; finally, a high-purity product is obtained through directional recrystallization of an ethanol-water mixed solvent. Competitive bromination and Grignard reagent application of a traditional route are fundamentally avoided, and the method has the remarkable advantages of being simple in route, mild in condition, safe to operate, high in selectivity, environmentally friendly and easy to implement industrially.

The application belongs to the field of medicine and chemical industry, and particularly relates to a preparation method of ketoprofen. 3-bromobenzoic acid is used as a starting material, and a chlorination reaction is carried out with thionyl chloride. Then, a Friedel-Crafts reaction is carried out with benzene under the catalysis of aluminum chloride. The reaction product is subjected to a Friedel-Crafts reaction with ethylene, an addition reaction with hydrobromic acid, a reaction with a cyanating agent, and then hydrolysis under the action of an acid, so as to obtain ketoprofen. The application provides a reasonable reaction route, realizes the preparation of ketoprofen by using cheap and readily available and green and environmentally-friendly reagents, avoids the use of highly corrosive, highly toxic, flammable and expensive reagents, has low requirements on equipment, reduces the operation difficulty and the burden of post-reaction treatment, and reduces the cost. The application is a simple, green and economic process route for preparing ketoprofen, the obtained product has high yield and good purity, and is suitable for industrial mass production of ketoprofen.

The application relates to the field of medicine synthesis, in particular to a three-step preparation method of a ketoprofen general compound. The ketoprofen general compound is prepared through three-step reactions of deamination, deesterification and acid hydrolysis from a prepared compound of formula IV, wherein R1 is -CONR4R5, -COX1, -COOR2 or -CN at the ortho position or the para position of an amine group, R2, R3, R4 and R5 are the same or different and are H or C1-C6 alkyl, and X1 is F, Cl, Br or I. The reaction is suitable for industrial production.

This invention provides a method for preparing loxoprofen acid, relating to the field of biomedical technology. The method involves mixing compound 1, 1-(1-pyrrolidine)cyclopentene, and an organic solvent, performing a condensation reaction, and then hydrolyzing the mixture under acidic conditions to obtain loxoprofen acid; wherein X is a halogen, and R includes -CN or -CONH2. This invention uses compound 1 and 1-(1-pyrrolidine)cyclopentene as starting materials, and prepares loxoprofen acid through a condensation reaction followed by hydrolysis under acidic conditions. The product yield is high, the purity is high, and continuous production of loxoprofen acid is possible. The operation is simple, generates little waste, is environmentally friendly, and has low production costs, making it suitable for industrial production. Furthermore, the preparation method provided by this invention concentrates the solvent after the condensation reaction to allow for subsequent hydrolysis, eliminating the need for separation and purification of the intermediate obtained from the condensation reaction, simplifying the operation steps, generating less waste, and being environmentally friendly.

The application discloses a continuous hydrolysis and extraction purification integrated process of 3-isobutyl glutaric acid, and relates to the technical field of 3-isobutyl glutaric acid. A micro-channel hydrolysis reaction liquid is generated; a high-dispersion acidification mixed liquid is obtained; a high gravity continuous mass transfer and liquid-liquid separation are carried out by using a high-speed rotating centrifugal field, a primary organic extraction phase rich in a target product is extracted; liquid-liquid complex washing is carried out under pulse oscillation, and a purified extraction phase is obtained; organic extraction solvent is gasified and stripped, and a supersaturated liquid material without solvent residue is collected at the bottom; under a multi-stage programmed cooling gradient, nucleation and crystal growth are induced, and a high-purity 3-isobutyl glutaric acid product is extracted after online solid-liquid separation. The application significantly improves the generation quality of a target intermediate and the robustness of a reaction system.

The invention discloses a synthesis method of 2, 4, 5-trifluorophenylacetic acid, and relates to the technical field of organic chemical industry, 2, 4-dichloro-5-fluorobenzoyl chloride is firstly subjected to cyanation to generate 2, 4-dichloro-5-fluorobenzoyl nitrile, then the 2, 4-dichloro-5-fluorobenzoyl nitrile and potassium fluoride are subjected to halogen exchange reaction in the presence of a phase transfer catalyst to generate 2, 4, 5-trifluorobenzoyl nitrile, and the 2, 4, 5-trifluorophenylacetic acid is obtained. The 2, 4, 5-trifluorophenylacetic acid is prepared from 2, 4, 5-trifluorophenylacetic acid and 2, 4, 5-trifluorophenylacetic acid as raw materials, then reduction is performed under p-toluenesulfonhydrazide and sodium borohydride, and hydrolysis is performed under an acidic condition to generate 2, 4, 5-trifluorophenylacetic

A process is described for preparing the compound of formula (S)-3 for optical enzymatic or chiral amine resolution of compounds of formula 4 wherein R is a cyano, carboxy or C1-C6 alkoxy carbonyl group and P is a protecting group of the hydroxy group.

The invention relates to application of a metal catalyst in catalytic hydrolysis of o-chlorophenylacetonitrile or phenylacetic acid, and the metal catalyst is a metal oxide of a manganese element and / or a cerium element, and / or a solid composite metal oxide containing a rare earth element and at least one of the manganese element, the cerium element, an alkali metal element and an alkaline earth metal element, and / or a solid composite oxide containing at least two rare earth elements. The metal catalyst provided by the invention has an efficient catalytic hydrolysis effect on chlorophenylacetonitrile or phenylacetic acid, and can achieve the purpose of efficient and environment-friendly preparation of chlorophenylacetic acid or phenylacetic acid.

The application belongs to the technical field of organic synthesis chemistry, and particularly relates to a fluorine-containing hydroxybenzoic acid compound and a preparation method. The application provides a novel synthesis path, which takes 4-fluoro-3-methoxybenzonitrile as a starting material, firstly performs specific demethylation reaction in benzene or toluene solvent through anhydrous aluminum chloride catalysis to obtain an intermediate 4-fluoro-3-hydroxybenzonitrile; then performs acid hydrolysis reaction on the intermediate in a mixed medium of concentrated sulfuric acid and water to convert the cyano group into a carboxyl group, and obtains 3-hydroxy-4-fluorobenzoic acid crude product; finally, high-purity product is obtained through directional recrystallization of an ethanol-water mixed solvent. The application fundamentally avoids competitive bromination and Grignard reagent application of a traditional route, and has the remarkable advantages of simple route, mild condition, safe operation, high selectivity, environmental friendliness and easy industrial implementation.

The invention relates to a preparation method of an aromatic cyclic carboxylic acid intermediate compound I. The preparation method comprises the following steps: S1, reacting with a ketal reagent under the catalysis of acid to prepare a compound as shown in a formula II; s2, reacting under an alkaline condition, and treating with acid to obtain a compound I; wherein X is an optionally substituted aromatic ring, and the aromatic ring is selected from a benzene ring, a thiophene ring and a naphthalene ring; the substituent group of the aromatic ring is selected from methyl, ethyl, propyl, butyl, amyl and isopropyl, preferably methyl; aromatic rings are selected from R1 and are independently selected from carbonyl protecting groups; or in the formula II, R1-R1 and atoms connected with the R1-R1 form a ring, and-R1-R1-is selected from carbonyl protecting groups; r1 is independently selected from a methyl group, an ethyl group, a benzyl group, a propyl group, a butyl group, a amyl group, an isopropyl group and a methylthio group; or R1-R1 cyclizes together with the atom to which they are attached, selected from the group consisting of R1-R1

The invention discloses a synthesis method of isopentenoic acid and isopentenoic acid ester, which comprises the following steps of: reacting isobutylene chloride and cyanide salt serving as raw materials to generate 3-methyl-3-butenenitrile, isomerizing the 3-methyl-3-butenenitrile into 3-methyl-2-butenenitrile, and hydrolyzing or alcoholyzing the 3-methyl-2-butenenitrile under an acidic condition to generate ammonium salt and the isopentenoic acid or the isopentenoic acid ester; and carrying out a series of treatment to obtain an isopentenoic acid product or an isopentenoic acid ester product. The method has the beneficial effects that the isobutene chloride and the cyanide salt which are low in price and easy to obtain are used as main raw materials, the raw materials are efficiently converted into the isopentenoic acid and the ester thereof, the production cost can be greatly reduced, the problem that the raw materials are limited in a traditional method can be solved, the target product isopentenoic acid and the ester thereof with relatively high purity can be obtained at high yield, and the method is suitable for industrial production. Few three wastes are generated in the synthesis process, and the generated three wastes are easy to treat, so that the environmental pollution can be reduced; the synthesis method is mild in condition and simple to operate, and is a production method for isopentenoic acid and ester thereof, which can realize large-scale industrial production.

The invention relates to the technical field of synthesis of medical intermediates, in particular to a preparation method of a synthetic intermediate of sodium N-(8-[2-hydroxybenzoyl]-amino) caprylate, which comprises the following steps: taking a compound 1 as a raw material, generating a halogenated product compound 2 under the action of a halogenating agent, cyaniding to obtain a compound 3, increasing a carbon chain, and purifying to obtain the intermediate of sodium N-(8-[2-hydroxybenzoyl]-amino) caprylate. Hydrolyzing the compound 3 under an alkaline condition to generate a compound 4, then dehydrating under the action of a catalyst to obtain a compound 5, performing ammoniation ring opening on the compound 5 to obtain a compound 6, then dehydrating to generate a compound 7, and finally generating a final product compound 8 under the action of a reducing agent. The preparation method has the advantages of easily available raw materials, safe and efficient reaction operation, good route selectivity, mild conditions, simple purification, high atom economy and high yield, and is suitable for industrial large-scale production.

This provides a new synthetic route and a new synthetic intermediate for N-(3-(6-amino-5-(2-(N-methylacrylamide)ethoxy)pyrimidine-4-yl)-5-fluoro-2-methylphenyl)-4-cyclopropyl-2-fluorobenzamide. [Solution] A synthesis method comprising converting compound X6b and compound F6 to compound F7, wherein: TIFF2026082843000085.tif54170 A synthesis method is provided in which X and Y are independently Cl, Br, or I, and P is an amine protecting group.

The application provides a preparation method of 2-chloro-6-sulfhydryl benzoic acid. Specifically provided is a preparation method of 2-chloro-6-sulfhydryl benzoic acid, which comprises the following steps: mixing a divalent palladium catalyst, a phosphine ligand, an alcohol solvent and an aromatic solvent in a protective atmosphere, adding water to pre-activate to obtain a reaction liquid; mixing the reaction liquid, a compound 2, 6-dichlorobenzoic acid, a sulfuration reagent and an inorganic base in a protective atmosphere to perform a sulfuration reaction, adding a reducing metal and an acid to react to obtain 2-chloro-6-sulfhydryl benzoic acid. The preparation method provided by the application is simple in operation, high in yield and capable of being scaled up to industrial production.

The present invention relates to the technical field of drug synthesis, and in particular to a method for synthesizing 2,2-dimethylpentanedioic acid. The method comprises the following steps: (1) uniformly mixing isobutyraldehyde, acrylonitrile, and tetrahydrofuran, cooling the mixture to 0-5°C, dropwise adding a sodium hydroxide aqueous solution, then carrying out a reaction while maintaining the temperature, heating to 50-55°C for a reaction, and separating a cyanoaldehyde intermediate; (2) uniformly mixing the cyanoaldehyde intermediate, water, and potassium dihydrogen phosphate, cooling the mixture to 0-5°C, and adding hydrogen peroxide; and dropwise adding a sodium chlorite aqueous solution, then heating to 23-28°C, carrying out a reaction while maintaining the temperature, dropwise adding a sodium bisulfite aqueous solution to quench the reaction, and separating a cyanic acid intermediate; and (3) uniformly mixing the cyanic acid intermediate with sulfuric acid, heating the mixture to 95-100°C while stirring, carrying out a reaction while maintaining the temperature, cooling to room temperature, and separating a crude 2,2-dimethylpentanedioic acid product; and adding cyclohexane for crystallization to obtain a product. The synthesis route of the present invention is simple and novel, the raw materials used have low prices, the synthesis method is simple and convenient to operate, and the product yield is relatively high.