36 results about "2-methylpropanoic acid" patented technology

The present invention discloses preparation of a 248 nm deep ultraviolet photoresist film forming resin based on a RAFT polymerization method, and belongs to the field of deep ultraviolet photoresists. According to the photoresist film forming resin, mainly 2-(dodecyl trithiocarbonate-yl)-2-methylpropanoic acid is adopted as a RAFT reagent, 4-acetoxy styrene, styrene, tert-butyl acrylate and 2-methyl-2-methacrylic acid adamantine ester are adopted as copolymerization monomers, 1-methoxy-2-propyl acetate is adopted as a reaction solvent to carry out solution polymerization under the condition of a free radical initiator so as to synthesize a low molecular weight distribution copolymer, a certain amount of sodium methoxide and methanol are added to carry out alcoholysis so as to obtain the copolymer having high transparency at 248 nm, and the copolymer is finally applied in the 248 nm photoresist. According to the present invention, the preparation is simple, the reaction conditions are mild, the molecular weight distribution of the obtained copolymer is narrow, the molecular weight can be well controlled, and the resin is suitable for 248 nm deep ultraviolet exposure.

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 advantages of high yield, freeness of meta-isomers and amide impurities, little pollution and applicable industrial production.

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 preparing zofenopril calcium. N-acetyl-L-oxyproline is adopted as a raw material. The method includes: a step of subjecting the N-acetyl-L-oxyproline and methanol to esterification, subjecting the obtained product and paratoluensulfonyl chloride to sulfonation, and subjecting the obtained product and thiophenol prepared from a sodium thiophenolate solution to thiophenyl substitution; a step of hydrolyzing the obtained product into an free acid by utilization of an alkali, performing recrystallization for purification, and performing deacetylation with hydrochloric acid to obtain (cis)-4-thiophenyl-L-proline hydrochloride; a step of reacting (S)-3-(benzoyl sulfhydryl)-2-methylpropanoic acid with thionyl chloride to obtain (S)-3-(benzoyl sulfhydryl)-2-methyl propionylchloride; a step of reacting the (S)-3-(benzoyl sulfhydryl)-2-methyl propionylchloride with the (cis)-4-thiophenyl-L-proline hydrochloride to obtain the free acid zofenopril; and a step of forming a potassium salt, purifying and reacting with a calcium chloride to obtain a calcium salt, thus obtaining a final product zofenopril calcium. The method has characteristics of easily available raw materials, simple preparation method, mild conditions, easy control, reasonable monitoring points in the preparation process, effective removal and control of impurities, capability of producing the final product with the needed crystal form preferentially in a high ratio, suitability for industrial production and large application value.

The invention provides a method for synthetizing Zofenopril Calcium salt, which takes N-acetyl-L-oxyproline as raw materials; the N-acetyl-L-oxyproline and methanol are esterified, paratoluensulfonyl chloride is sulphonated, and thiophenyl is substituted; the obtained product is hydrolyzed to be freeacid by alkali, and (cis form)-4-thiophenyl-L-proline hydrochloride is further obtained by hydrochloric acid deacetylation reaction; in addition, (S)-3-(benzoyl sulfhydryl group)-2-methylpropanoic acid reacts with thionyl chloride, and (S)-3-(benzoyl sulfhydryl group)-2-methyl propionyl chloride which then reacts with the (cis form)-4-thiophenyl-L-proline hydrochloride, so that Zofenopril freeacid is obtained; the Zofenopril freeacid is firstly made into sylvite, and then refined and purified to be calcium salt, so that the termination product is obtained. The materials of the method of the invention is easily obtained, the process route is simple, and the reaction conditions are mild; therefore, the method is easy to operate and suitable for commercial process.

The invention discloses a method for preparing a S-(-)-Benzoylthio-2-methylpropanoic acid compound. S-(-)-3-acetylthio-2-methylpropionic acid as a raw material shown in the formula II is hydrolyzed ina reacting solvent to obtain S-(-)-3-mercapto-2-methylpropionic acid shown in hte formula III, and the S-(-)-3-mercapto-2-methylpropionic acid and benzoyl chloride are subjected to condensation to obtain the S-(-)-Benzoylthio-2-methylpropanoic acid shown in the formula I. The preparation method is easy in operation, the raw materials and accessory materials are low in cost and easy to obtain, thereaction conditions are mild, the yield is high, and the quality is high. (The formula is shown in the description.).

The invention relates to the field of sterilization and disinfection, and particularly relates to low corrosive oxidation potential sterilization water and a preparation method thereof. The preparation method of the low corrosive oxidation potential sterilization water comprises the following steps: (1) providing an available chlorine provision unit which contains available chlorine or can generate available chlorine; (2) providing a pH value regulation unit; and (3) mixing the pH value regulation unit and the available chlorine provision unit to obtain a strong oxidizing solution, wherein the pH value of the strong oxidizing solution is 2-8, the oxidation-reduction potential is not lower than 600 mV, the available chlorine content is not lower than 3 mg/L, and the sum of the 2-methylpropanoic acid content and the 2-methylpropionate ion content is not higher than 1.8 mol/L. Compared with the existing acidic oxidation potential sterilization water, the sterilization water prepared by the oxidation potential sterilization water preparation method can reduce the corrosion to metal, thereby widening the application range.

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 synthetic method of a 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 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 and adjusting pH to obtain 2-(4-cyclopropoxycarbonylphenyl)-2-methylpropanoic acid; reacting the 2-(4-cyclopropoxycarbonylphenyl)-2-methylpropanoic acid in HCl for 20-30h at 60-100 DEG C and recrystallizing to obtain 2-[4-(4-chlorobutyryl)phenyl]-2-methylpropanoic acid; adding the 2-[4-(4-chlorobutyryl)phenyl]-2-methylpropanoic acid in the hydrochloric acid solution of absolute alcohol to prepare the 2-[4-(4-chlorobutyryl)phenyl]-2-methacrylate, and finally obtaining the target product of the invention through routine techniques. The invention has the advantages of high yield, freeness of meta-isomers and amide impurities, little pollution and applicable industrial production.

Selective bromination of 2-methyl-2-phenylpropanoic acid in aqueous medium is described to obtain pure 2-(4-bromophenyl)-2-methylpropanoic acid, which is a useful key intermediate in the process of manufacturing pure fexofenadine.

The invention discloses a synthetic method of 2, 3-dibromo-2-methylpropanoic acid, which takes methacrylic acid and bromine as raw materials and comprises the following steps of: 1) adding bromine into methacrylic acid water solution, reacting for 1h to 5h at the temperature of 50 to 100 DEG C, and obtaining crude product solution of 2, 3-dibromo-2-methylpropanoic acid; wherein the mol ratio of methacrylic acid and bromine is 1: 1 to 1: 3; 2) obtaining mother liquid and solid by carrying out temperature reduction and crystallization, and filtration; and 3) obtaining the 2, 3-dibromo-2-methylpropanoic acid by washing the solid for 2 to 3 times, and drying. The method for producing 2, 3-dibromo-2-methylpropanoic acid has the advantages of high yield coefficient, environmental protection and the like.

The invention discloses a method for synthesizing 2-[4-(4-chlorobutyryl)phenyl]-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 for 20-40h, and adjusting pH to be 3 by hydrochloric acid, extracting, drying and filtering to obtain 2-(4-cyclopropoxycarbonylphenyl)-2-methylpropanoic acid, and adding the 2-(4-cyclopropoxycarbonylphenyl)-2-methylpropanoic acid in an inorganic acid, reacting for 20-30h at 60-100 DEG C, extracting, drying, filtering and crystallizing by ethanol to obtain the product target. The invention has a simple technology, high yield and little pollution.