55results 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 present invention provides a method for preparing the active pharmaceutical ingredient of fenfluramine. Aspects of the present invention include (a) hydrolyzing a 2-(3-(trifluoromethyl)phenyl)acetonitrile composition to produce a 2-(3-(trifluoromethyl)phenyl)acetic acid composition; (b) reacting the 2-(3-(trifluoromethyl)phenyl)acetic acid composition with acetic anhydride and a catalyst to prepare a 1-(3-(trifluoromethyl)phenyl)propan-2-one composition; and (c) reducing and aminating the 1-(3-(trifluoromethyl)phenyl)propan-2-one composition with a borohydride reducing agent and ethylamine to produce a fenfluramine composition. The present invention also provides a composition and a pharmaceutical ingredient comprising a pharmaceutically acceptable salt of fenfluramine prepared according to the method and having less than a total of 0.2% by weight of trifluoromethyl regioisomers.

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 present invention relates to a catalyst and a preparation method thereof. The catalyst comprises a mesoporous γ-Al2O3 / SiO2 support and an active component supported on the support. The active component is a complex formed by a metal salt and a modifier. The modifier is a reaction product of a first component selected from organic acids and / or inorganic acids and a second component selected from organic bases. The catalyst is weakly acidic. The present invention also relates to a method for synthesizing malonic ester compounds, comprising: mixing cyanoacetic acid, water and the catalyst and performing an activation treatment, then carrying out a hydrolysis reaction on the first mixed material obtained by the activation treatment in the presence of a catalyst for cyanoacetic acid hydrolysis reaction, and then adding an alcohol to the second mixed material obtained by the hydrolysis reaction to carry out an esterification reaction to obtain malonic ester compounds. The catalyst of the present invention can effectively solve problems such as low yield, serious equipment corrosion, and large amounts of "three wastes", and environmentally friendly and efficiently realizes the synthesis of malonic ester compounds.

The present invention relates to the technical field of organic chemistry, and discloses a preparation method of 9-phenanthrene formic acid, wherein the preparation method comprises the following steps: using phenanthrene as a main raw material, iron bromide or zinc bromide as a catalyst, reacting with hydrobromic acid and hydrogen peroxide at 20 to 50 ° C to generate 9-bromophenanthrene, 9-bromophenanthrene reacts with cyanide under a catalyst to generate 9-nitrile phenanthrene, and then hydrolyzing under alkaline conditions to obtain 9-phenanthrene formic acid. The present invention uses cheap and readily available raw materials such as phenanthrene, hydrobromic acid, hydrogen peroxide and sodium cyanide to prepare 9-phenanthrene formic acid, with low production cost, high conversion rate, good product quality, mild reaction conditions, low equipment requirements, and can be used for large-scale industrial preparation of 9-phenanthrene formic acid.

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 discloses a preparation method of 2-methyl-4-acetylbenzoic acid, and relates to the technical field of production of 2-methyl-4-acetylbenzoic acid. 1-(4-fluoro-3-methylphenyl) ethanone is obtained from o-fluorotoluene and acetyl chloride under the catalytic action of AlCl and sulfonic acid functionalized mesoporous silica; the preparation method comprises the following steps: preparing 4-acetylbenzonitrile from 4-methylbenzonitrile under the action of a supported metal catalyst, then obtaining 4-acetyl-2-methylbenzonitrile under the action of 15-crown ether-5, PEG-400 and acetone cyanohydrin matched with CuI, and finally obtaining 2-methyl-4-acetylbenzoic acid under the action of oxygen and the supported metal catalyst. And the product has high yield and purity and is environment-friendly.

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 invention relates to an industrial preparation method for synthesizing p-hydroxyphenylacetic acid through copper / ligand catalysis. Specifically, the invention discloses a preparation method for preparing p-hydroxyphenylacetic acid by taking p-chlorobenzyl cyanide as a raw material in an inert solvent and carrying out carbon-oxygen bond coupling reaction under the action of a catalyst and alkali, the method is simple to operate and high in product yield and purity, the production cost is greatly reduced, and the method is very easy for industrial production.

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 relates to a post-treatment method of a high-purity ester compound, reaction liquid of hydrolysis reaction and esterification reaction is treated through simple operation, high-purity by-products can be recycled, the ester compound with high purity and yield can be obtained, the post-treatment method is simple and convenient to operate, emission of three wastes is greatly reduced, and the method is suitable for industrial production. And large-scale industrial production is facilitated.

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.

The invention discloses a synthetic method of fluorine-containing polyester monomer dicarboxylic acid, which comprises the following steps: taking 2, 2-bis (4-aminophenyl) hexafluoropropane as a raw material, carrying out diazotization and Sandmeyer reaction to obtain an intermediate I, and then carrying out carbonyl insertion reaction to obtain 2, 2-bis (4-carboxyphenyl) hexafluoropropane, or carrying out cyanation reaction on the intermediate I to obtain an intermediate II, and then carrying out carbonyl insertion reaction to obtain 2, 2-bis (4-aminophenyl) hexafluoropropane. And hydrolyzing to obtain the 2, 2-bis (4-carboxyl phenyl) hexafluoropropane. The synthesis method disclosed by the invention is simple and easy to operate, high in yield and high in product purity, and can be applied to actual 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 invention relates to the field of high polymer materials, and discloses a preparation method and application of high-temperature-resistant transparent modified polyamide. The preparation method comprises the following steps: 1) blending 9, 9-di-[(4-phenylphenoxy) dibenzoic acid] fluorene with diacid and diamine, and carrying out esterification reaction; and 2) carrying out condensation polymerization on the esterification product to obtain the high-temperature-resistant transparent modified polyamide with the glass transition temperature of more than 130 DEG C. According to the invention, 9, 9-di-[(4-phenylphenoxy) dibenzoic acid] fluorene is used as a modification monomer, and is copolymerized with other binary acid and diamine to synthesize the modified polyamide, and the modified polyamide not only has high transparency, but also still has good mechanical properties and dimensional stability at high temperature. Therefore, the high-temperature-resistant transparent modified polyamide is applicable to the application fields of optical films, optical lenses, reflective protective films, optical fibers or liquid crystal displays and the like.

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.