36 results about "2-methylpropanoic acid" patented technology

The refrigerating machine oil of the invention includes an ester of a polyhydric alcohol and a fatty acid, wherein the molar ratio of C4-C6 fatty acid and C7-C9 branched fatty acid in the fatty acid is between 15:85 and 90:10, the C4-C6 fatty acid includes 2-methylpropanoic acid, and the ratio of the total C4-C6 fatty acid and C7-C9 branched fatty acid in the total fatty acids composing the ester is at least 20 mol %. The working fluid composition for a refrigerating machine according to the invention comprises the refrigerating machine oil, a difluoromethane refrigerant and / or an unsaturated fluorinated hydrocarbon refrigerant.

This refrigerating machine oil comprises esters of a polyhydric alcohol with fatty acids. In the fatty acids, the molar ratio of C4-6 fatty acids to branched C7-9 fatty acids is 15:85 to 90:10, and the C4-6 fatty acids contain 2-methylpropanoic acid, with the sum total of the C4-6 fatty acids and the branched C7-9 fatty acids accounting for at least 20 mol% of the whole of the fatty acids constituting the esters. This working fluid composition for refrigerating machines comprises the refrigerating machine oil and a difluoromethane refrigerant and / or an unsaturated fluorinated hydrocarbon refrigerant.

The invention discloses a method for synthesizing an alecensa hydrochloride intermediate 2-(4-ethyl-3-iodophenyl)-2-methylpropanoic acid. The method is characterized by comprising steps of carrying out Friedel-Crafts reaction on ethylbenzene and 3-halogen-2-methyl-1-propylene to obtain 1-halogn-2-(4-ethyl phenyl)-2-methylpropane; carrying out reaction on the 1-halogn-2-(4-ethyl phenyl)-2-methylpropane and magnesium to obtain 2-(4-ethyl phenyl)-2-methyl propyl magnesium halide; carrying out reaction on the 2-(4-ethyl phenyl)-2-methyl propyl magnesium halide and oxygen to obtain 2-(4-ethyl phenyl)-2-methyl-1-propyl alcohol; oxidizing the 2-(4-ethyl phenyl)-2-methyl-1-propyl alcohol, sodium hypochlorite and sodium chlorite by the aid of 2,2,6,6-tetramethyl piperidine oxide to obtain 2-(4-ethyl phenyl)-2-methylpropanoic acid; carrying out reaction on the 2-(4-ethyl phenyl)-2-methylpropanoic acid and iodine in the presence of oxidizing agents under acidic conditions to obtain the alecensa hydrochloride intermediate. 2-(4-ethyl-3-iodophenyl)-2-methylpropanoic acid. The 2,2,6,6-tetramethyl piperidine oxide is used as a catalyst. The method has the advantages that the method is easy and convenient to operate, high in yield, low in cost and little in pollution, raw materials for the alecensa hydrochloride intermediate 2-(4-ethyl-3-iodophenyl)-2-methylpropanoic acid are inexpensive and are easily available, and industrial production can be facilitated.

The invention discloses a preparation method of an alectinib intermediate, tert-butyl 4-{4-ethyl-3-[4-(morpholine-4-yl)piperidine-1-yl]phenyl}-4-methyl-3-oxovalerate. The preparation method comprises: subjecting ethyl 2-(4-ethyl-3-hydroxyphenyl)acetate and triflic anhydride to triflic acid esterification; subjecting the obtained 5-[(ethoxycarbonyl)methyl]-2-ethylphenyltriflate and 4-(4-piperidyl)morpholine to substitution reaction; subjecting the obtained ethyl 2-{4-ethyl-3-[4-(morpholine-4-yl)piperidine-1-yl]phenyl}acetate and methyl iodide to bis-methylation reaction; hydrolyzing the obtained ethyl 2-{4-ethyl-3-[4-(morpholine-4-yl)piperidine-1-yl]phenyl}-2-methylpropanoate; subjecting the obtained 2-{4-ethyl-3-[4-(morpholine-4-yl)piperidine-1-yl]phenyl}-2-methylpropanoic acid and mono-tert-butyl malonate to condensation reaction to obtain the alectinib intermediate. The preparation method is simple to perform and low in cost, is a green technique and is applicable to industrial production.

The invention discloses a preparation method of an alectinib intermediate, tert-butyl 4-{4-ethyl-3-[4-(morpholine-4-yl)piperidine-1-yl]phenyl}-4-methyl-3-oxovalerate. The preparation method comprises: subjecting ethyl 2-(4-ethyl-3-hydroxyphenyl)acetate and triflic anhydride to triflic acid esterification; subjecting the obtained 5-[(ethoxycarbonyl)methyl]-2-ethylphenyltriflate and 4-(4-piperidyl)morpholine to substitution reaction; subjecting the obtained ethyl 2-{4-ethyl-3-[4-(morpholine-4-yl)piperidine-1-yl]phenyl}acetate and methyl iodide to bis-methylation reaction; hydrolyzing the obtained ethyl 2-{4-ethyl-3-[4-(morpholine-4-yl)piperidine-1-yl]phenyl}-2-methylpropanoate; subjecting the obtained 2-{4-ethyl-3-[4-(morpholine-4-yl)piperidine-1-yl]phenyl}-2-methylpropanoic acid and mono-tert-butyl malonate to condensation reaction to obtain the alectinib intermediate. The preparation method is simple to perform and low in cost, is a green technique and is applicable to industrial production.

The refrigerating machine oil of the invention includes an ester of a polyhydric alcohol and a fatty acid, wherein the molar ratio of C4-C6 fatty acid and C7-C9 branched fatty acid in the fatty acid is between 15:85 and 90:10, the C4-C6 fatty acid includes 2-methylpropanoic acid, and the ratio of the total C4-C6 fatty acid and C7-C9 branched fatty acid in the total fatty acids composing the ester is at least 20 mol %. The working fluid composition for a refrigerating machine according to the invention comprises the refrigerating machine oil, a difluoromethane refrigerant and / or an unsaturated fluorinated hydrocarbon refrigerant.

The invention relates to a method for synthesizing an aztreonam compound. The method comprises the following steps of: (1) adding water and a water-soluble non-aqueous solvent into a reaction container, adding trans-3(S)-amino-4-methyl-2-keto-1-azetidine sulfonic acid, triethylamine and (Z)-2-[(2-aminothiazole-4-radical)-(benzothiazole-2-sulfenyl carbonyl) methylamine oxygroup]-2-methylpropanoic acid tert-butyl ester for reacting, and adjusting the pH with acid and separating crystals out to obtain tertiary butyl aztreonam; and (2) subjecting the tertiary butyl aztreonam and acid-water mixed liquor to reaction and performing post-treatment to obtain aztreonam. By adopting the method, the reaction time can be shortened, the reaction speed can be increased, the production cost can be lowered, and environmental pollution can be reduced.

The invention discloses a preparation method of an antiallergic agent fexofenadine hydrochloride, comprising the steps of adding an alkali metal hydroxide in an alcohol solvent, dripping N-methyl-N-methoxyl-2-[4-(4-chlorobutyryl)phenyl]-2-methacrylamide alcohol solvent in the solvent, reacting for 10-30h at 20-50 DEG C, conventionally processing to obtain N-methyl-N-methoxyl-2-(4-cyclopropoxycarbonylphenyl)-2-methacrylamide; adding the N-methyl-N-methoxyl-2-(4-cyclopropoxycarbonylphenyl)-2-methacrylamide in an inorganic acid, reacting for 20-30h at 60 DEG C, conventionally processing and crystallizing by ethanol to obtain 2-[4-(4-chlorobutyryl)phenyl]-2-methylpropanoic acid; adding the 2-[4-(4-chlorobutyryl)phenyl]-2-methylpropanoic acid in the alcohol solvent in which HCl gas is infused,conventionally processing to obtain 2-[4-(4-chlorobutyryl)phenyl]-2-methacrylate, and finally obtaining the target product of the invention through routine techniques. The invention has the advantagesof high yield, freeness of meta-isomers and amide impurities, little pollution and applicable industrial production.

The invention discloses a method for synthesizing 2-[4-(4-chlorobutyryl)phenyl]-2-methacrylate, comprising the steps of adding an alkali metal hydroxide in an alcohol solvent, dripping N-methyl-N-methoxyl-2-[4-(4-chlorobutyryl)phenyl]-2-methacrylamide alcohol solvent in the solvent, reacting for 10-30h at 20-50 DEG C, extracting, drying, and filtering to obtain N-methyl-N-methoxyl-2-(4-cyclopropoxycarbonylphenyl)-2-methacrylamide; adding the N-methyl-N-methoxyl-2-(4-cyclopropoxycarbonylphenyl)-2-methacrylamide in an inorganic acid, reacting for 20-30h at 60 DEG C, extracting, drying, filtering, crystallizing by ethanol to obtain 2-[4-(4-chlorobutyryl)phenyl]-2-methylpropanoic acid; infusing HCl gas in the alcohol solvent, then adding the 2-[4-(4-chlorobutyryl)phenyl]-2-methylpropanoic acid, washing by water, drying and filtering to obtain the target product. The synthetic method of the invention has high yield, little pollution and applicable industrial production.

The invention discloses a method for synthesizing 2-[4-(4-chlorobutyryl)phenyl]-2-methacrylate, comprising the steps of adding an alkali metal hydroxide in an alcohol solvent, dripping N-methyl-N-methoxyl-2-[4-(4-chlorobutyryl)phenyl]-2-methacrylamide alcohol solvent in the solvent, reacting for 10-30h at 20-50 DEG C to obtain N-methyl-N-methoxyl-2-(4-cyclopropoxycarbonylphenyl)-2-methacrylamide; refluxing the N-methyl-N-methoxyl-2-(4-cyclopropoxycarbonylphenyl)-2-methacrylamide in an alkaline alcohol solvent for 20-40h and adjusting pH to be 3 so as to obtain 2-(4-cyclopropoxycarbonylphenyl)-2-methylpropanoic acid; reacting the 2-(4-cyclopropoxycarbonylphenyl)-2-methylpropanoic acid in an inorganic acid for 20-30h at 60-100 DEG C and recrystallizing to obtain 2-[4-(4-chlorobutyryl)phenyl]-2-methylpropanoic acid; and finally adding the 2-[4-(4-chlorobutyryl)phenyl]-2-methylpropanoic acid in the hydrochloric acid solution of absolute alcohol, and reacting for 3h at 60 DEG C to obtain the target product. The preparation method has high product yield, little pollution and applicable industrial product.

The invention discloses a process for preparing sulindac comprising the steps of, condensating 4-fluorobenzyl chloride and diethyl methylmalonate at the presence of organic base, obtaining 2-(4-fluorobenzyl)-2-diethyl methylmalonate, hydrolyzing in aqueous alkali to obtain 2-(4-fluorobenzyl)-2-methyl malonic acid, carrying out decarboxylation directly under high temperature to obtain 3-(4-fluorophenyl)-2-methylpropanoic acid, chlorinating with sulfoxide acyl chloride, then using aluminium trichloride or waterless zinc chloride as catalyst, carrying out F-C acylation to obtain 6-fluoro-2-methylindanone, condensing with cyanocetic acid, hydrolyzing to obtain 5-fluoro-methyl-3-indenes acetic acid, then condensing with p-methylthiobenzaldehyde to obtain 5-fluoro-2-methyl-1-(4-methylthiobenzal)-3-indenes acetic acid, finally using organic acid as solvent, peracid or hydroperoxide as oxidation agent to obtain the sulindac.

The invention provides a method for synthesizing 2-methyl propionate-[(2S)-4-(2,4-diflurophenyl)-2-hydroxymethyl-4-amylene-1-group] ester.The method includes the steps that 1,2,3-trichloropropane is added dropwise to 1,3-difluorobenzene, and aluminum trichloride is added for a reaction; the mixture is added to a hydrochloric acid solution for extraction, and washing is conducted with a saturated NaHCO3 solution, water and saturated salt solution in sequence; anhydrous Na2SO4 is used for drying and filtering, evaporation is conducted for solvent removal, and 1,3-dichloro-2-(2,4-diflurophenyl) propane is obtained; 1,3-dichloro-2-(2,4-diflurophenyl) propane and potassium hydroxide are added to tert butyl alcohol, and reflux is conducted for 3.5-6 h; tert butyl alcohol is removed, ice water is added, the mixture is neutralized with hydrochloric acid at the temperature of 5 to -5 DEG C to be neutral, dichloromethane is used for three times of extraction, anhydrous Na2SO4 is used for drying and filtering, a distillation product is dissolved in DMSO, a product obtained after diethyl malonate and diethyl malonate react are added and a product obtained after lithium chloride and sodium borohydride react are added and dissolved in methylbenzene, and sodium bicarbonate, Novo SP 435 esterifying enzymes and isobutyric anhydride are added for a reaction; the target product is obtained after washing, crystallization and drying are conducted.The synthesis path is shown in the description.

The invention relates to a synthesis method of ciprofibrate. In the synthesis method, acetic acid-4-(2,2-dichlorocyclopropyl) phenyl ester is adopted as a raw material, and 2-[4-(2,2-dichlorocyclopropyl) phenoxy]-2-methylpropanoic acid is obtained through alcoholysis, alkylation and alkaline hydrolysis processes. The synthesis method of ciprofibrate, provided by the invention, has the benefits that the raw materials used in the whole reaction are inexpensive and easy to get, the reaction conditions are mild, the operation is convenient, the yield is good, all solvents used in the reaction can be recycled, and the environmental pollution degree is low.

The invention discloses a method for synthesizing 2-(4-cyclopropoxycarbonylphenyl)-2-methylpropanoic acid, comprising the steps of adding an alkali metal hydroxide in an alcohol solvent, dripping the alcohol solvent of N-methyl-N-methoxyl-2-[4-(4-chlorobutyryl)phenyl]-2-methacrylamide in the alcohol solvent, agitating and reacting for 10-30h at 20-50 DEG C, extracting, drying and filtering to obtain N-methyl-N-methoxyl-2-(4-cyclopropoxycarbonylphenyl)-2-methacrylamide; adding the N-methyl-N-methoxyl-2-(4-cyclopropoxycarbonylphenyl)-2-methacrylamide in the alcohol solvent of the alkali metal hydroxide, refluxing and reacting for 20-40h, and adjusting the pH of the reaction mixture to be 3 by hydrochloric acid, extracting, drying, filtering and removing methylene dichloride to obtain 2-(4-cyclopropoxycarbonylphenyl)-2-methylpropanoic acid. The synthetic method of the invention has the advantages of a few reaction steps, simple preparation technology, high yield, little pollution and lowproduction cost.

The invention discloses a method for synthesizing 2-[4-(4-chlorobutyryl)phenyl]-2-methylpropionic acid: adding alkali metal hydroxide to an alcohol solvent, and then adding N- Alcohol solution of methyl-N-methoxy-2-[4-(4-chlorobutyryl)phenyl]-2-methylpropionamide, react at 20~50°C for 10~30h, evaporate the solvent to dryness, Extract, dry, and filter to obtain N-methyl-N-methoxy-2-(4-cyclopropoxycarbonylphenyl)-2-methylpropionamide; then N-methyl-N-methoxy -2-(4-cyclopropoxycarbonylphenyl)-2-methylpropanamide is added to the mineral acid, the weight ratio of the two is 1:2~8, react at 60°C~100°C for 20~30h, extract, Dry, filter, and recrystallize to obtain the target product. The invention has the advantages of simple preparation process, high yield and little pollution.