93results about "Preparation from nitriles" patented technology

To provide a method for producing 4-ketobenzamide derivatives and 4-ketobenzoic acid derivatives.SOLUTION: The present invention provides a method for producing a 4-ketobenzamide compound represented by formula (2), by amidating a compound represented by formula (1), which is obtained through cyanation of a compound represented by formula (3), as well as a method for producing a 4-ketobenzoic acid derivative represented by formula (6), by hydrolyzing the compound represented by formula (1) or the compound represented by formula (2), and a method for producing a 4-ketobenzoic acid ester derivative represented by formula (5), by esterifying the compound represented by formula (2), wherein R1 represents a C1-C6 alkyl group or the like, R2 represents a C1-C6 alkyl group or the like, R3 represents a C1-C6 alkyl group or the like, X represents a halogen atom or the like, Y represents a C1-C6 alkyl group or the like, and n represents an integer of 0-3.SELECTED DRAWING: None

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 belongs to the field of chemical synthesis, and particularly relates to a preparation method of aromatic diether dicarboxylic acid, which comprises the following steps: (1) under the protection of inert gas, adding aromatic diphenol, p-fluorobenzonitrile, basic carbonate and a solvent 1 into a reactor, and reacting at 120-150 DEG C for 10-20 hours to obtain aromatic diether dinitrile; and (2) adding aromatic diether dinitrile, alkali metal hydroxide and a solvent 2 into the reactor, reacting at 100-150 DEG C for 10-20 hours, neutralizing with inorganic acid until the pH value is 1-2, filtering, washing with water until the pH value is neutral, and drying to obtain the product. By selecting specific reaction raw materials and process conditions, higher yield is successfully realized at lower temperature, and the method is very suitable for industrial production of aromatic diether dicarboxylic acid.

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.

Provided is a plasticizer composition to which a cyclohexane polyester-based substance is applied as a plasticizer in combination with a perhydride having a smaller number of ester groups than the cyclohexane polyester-based substance, so that volatile loss, thermal stability, and mechanical properties such as an elongation rate and tensile strength are improved.

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 utility model discloses malonic acid hydrolysis and distillation integrated equipment which comprises a kettle body, the bottom end of the kettle body is fixedly connected with a plurality of supporting legs, the top end of the kettle body is fixedly connected with a supporting frame, the middle of the supporting frame is in sliding clamping connection with a movable shaft, the bottom end of the movable shaft is coaxially and rotatably connected with a transmission rotating shaft, and the transmission rotating shaft is in sliding clamping connection with a transmission cylinder. The transmission cylinder is rotationally connected with the top of the kettle body, the top end of the transmission cylinder is fixedly sleeved with an outer gear ring, one side of the outer gear ring is meshed with a gear, the gear is fixedly connected with one side of a double-output-shaft motor, the end part of the other side of the double-output-shaft motor is fixedly connected with a cylindrical cam, and the cylindrical cam is in transmission connection with a movable shaft; and the two sides of the bottom end of the transmission rotating shaft are fixedly connected with scraping plates respectively, and the scraping plates are movably arranged in the kettle body. The double-output-shaft motor drives the cylindrical cam to rotate circumferentially, the cylindrical cam drives the movable shaft to do linear reciprocating motion, and the movable shaft drives the transmission rotating shaft which is rotationally connected to do synchronous linear reciprocating lifting motion.

The invention discloses a 2-hydroxy-benzonitrile kettle residue recovery treatment process, and belongs to the technical field of 2-hydroxy-benzonitrile. The process comprises the following steps: adding alkali liquor into the 2-hydroxy-benzonitrile production wastewater, adjusting the pH value of the wastewater, and adding montmorillonite for hydrolysis reaction to obtain a hydrolysis solution; adding an acid solution into the hydrolysis solution to adjust the pH value, stirring to separate out a solid, filtering, washing and drying to obtain salicylic acid; the method comprises the following steps: dissolving salicylic acid in deionized water, introducing a salicylic acid solution and ammonia water into a fixed bed reactor filled with a (BaHPO4) / C (at) A < l > 2O3 catalyst, and purifying a reaction product to obtain the 2-hydroxy-benzonitrile. Under the action of the (BaHPO4) / C (at) A < l > 2O3 catalyst, salicylic acid is converted to prepare the 2-hydroxy-benzonitrile, so that the environmental pollution caused by a large amount of residual wastewater in a 2-hydroxy-benzonitrile production reaction kettle is avoided, and the recycling of resources is realized.

Provided are processes for preparing substituted phenylacetonitriles and substituted phenylacetic acids. The processes disclosed herein provide phenylacetic acids or derivatives thereof in yields greater than 75 % as determined from the benzoic acid starting material and require less steps or hazardous agents and solvents than known methods. The substituted phenylacetic acids can find applications in the preparation of new active ingredients, such as in the field of diabetes, e.g., for GLP-1 receptor agonists.

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 provides a preparation method of 2-chloro-6-mercaptobenzoic acid. The 2-chloro-6-mercaptobenzoic acid is used as a raw material. Comprising the following steps: in a protective gas atmosphere, mixing a bivalent palladium catalyst, a phosphine ligand, an alcohol solvent and an aromatic solvent, and adding water for pre-activation to obtain a reaction solution; and in a protective gas atmosphere, mixing the reaction liquid, a compound 2, 6-dichlorobenzoic acid, a vulcanizing reagent and inorganic alkali, performing vulcanization reaction, and adding reducing metal and acid for reaction to obtain the 2-chloro-6-mercaptobenzoic acid. The preparation method provided by the invention is simple and convenient to operate and high in yield, and can be amplified to industrial production.

The present invention relates to a method for preparing substituted 4-(N'-hydroxycarbamimidoyl)benzoic acid, which can be obtained by hydration of substituted terephthalonitrile of formula II in an aqueous medium catalyzed by nitrilase to provide 4-cyanobenzoic acid (ammonium) IIa. After hydration, the aqueous reaction medium is treated with hydroxylamine or a salt thereof to provide amide oxime I.

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.

Methods of preparing a fenfluramine active pharmaceutical ingredient are provided. Aspects of the method 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 produce a 1-(3-(trifluoromethyl)phenyl)propan-2-one composition; and (c) reductively aminating the 1-(3-(trifluoromethyl)phenyl)propan-2-one composition with ethylamine using a borohydride reducing agent to produce a fenfluramine composition. Also provided are compositions and pharmaceutical ingredients prepared according to the subject methods including a pharmaceutically acceptable salt of fenfluramine and having less than 0.2% by weight in total of trifluoromethyl regioisomers.

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 discloses a synthesis method of p-fluorobenzoic acid, and relates to the technical field of chemical synthesis. According to the method, p-fluorobenzonitrile is adopted as a reaction raw material, p-fluorobenzoic acid is prepared through a fluorine-chlorine exchange and hydrolysis combined method, nitrobenzene and sulfolane are used as a mixed solvent in the fluorine-chlorine exchange process, it can be guaranteed that p-fluorobenzoic acid is synthesized within a short time, the yield of the synthesized p-fluorobenzoic acid is high, and the method is suitable for industrial production. The problems of serious environmental pollution, high raw material cost and low yield of p-fluorobenzoic acid synthesis in the prior art are solved.

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.