114 results about "Butyryl chloride" patented technology

The invention discloses a preparation method of spiromesifen, which uses 1-carboxyl cyclopentanol, 2, 4, 6-trimethylbenzene dichloroacetyl chloride and 3, 3-dimethyl butyryl chloride as main materials. The preparation method comprises (1), generating compound II: reacting 1-carboxyl cyclopentanol and 2, 4, 6-trimethylbenzene dichloroacetyl chloride in the presence of catalyst and in organic solvent, (2), generating compound III by heating the compound II and strong alkali in alcohol solution or in aprotic strong polar solvent to process reflux reaction, (3), generating spiromesifen by reacting the compound III and 3, 3-dimethyl butyryl chloride in the presence of catalyst and in organic solvent, wherein the prepared spiromesifen is represented as above. The preparation method of spiromesifen is suitable for industrial production.

The invention discloses a method used for preparing lopinavir using one-pot method. According to the method, under certain organic solvent conditions, (2S)-(1-Tetrahydropyramid-2-one)-3-methylbutanoicacid is reacted with thionyl chloride so as to obtain (2S)-(1-Tetrahydropyramid-2-one)-3-methyl butyryl chloride; a weak base acid binding agent and N-[(1S,2S,4S)-4-amino-2-hydroxy-5-phenyl-1-(phenylmethyl)pentyl]-2-(2,6-dimethylphenoxy)acetamide are added into an obtained reaction system for amidation reaction; after amidation reaction, an obtained product is subjected to post-treatment so as toobtain lopinavir finished product. According to the method, on-pot method is adopted, the process is simple, production period is short, the finial products can be separated and purified easily, synthesis yield is high, the method is economical and is high in feasibility, and is suitable for industrialized production.

The invention discloses a process method for synthesizing and purifying 4-chlorobutyryl chloride. The process method comprises the following steps of reacting gamma-butyrolactone and thionyl chloride in the presence of a mixed catalyst to synthesize a 4-chlorobutyryl chloride crude product and purifying the 4-chlorobutyryl chloride crude product to obtain the 4-chlorobutyryl chloride finished product of which the purity is equal to or greater than 99%, the individual impurity is less than 0.30% and the yield is equal to or greater than 90%. In the process method, exhaust gas generated in the production of 4-chlorobutyryl chloride is comprehensively utilized to produce a 30% hydrochloric acid and sodium sulfite solution and the tail material is used for producing 4-chlorobutyric acid ester. The process method is simple, convenient to operate, high in yield and purity of a product and almost free of emission of three wastes and is environmentally friendly.

The invention relates to an improved synthesis method for sex pheromone of euproctis pseudoconspersa, which is characterized in that 1, 7-heptanediol and 30-70 percent of hydrobromic acid solution react at the temperature of 50-130 DEG C and monobromide product 7-bromine-1-heptanol is obtained; the monobromide product 7-bromine-1-heptanol reacts with triphenyl phosphine in organic solvent I at the temperature of 50-130 DEG C, thus obtaining quaternary ammonium salt of triphenyl phosphine; with the function of organic base I or inorganic base, the obtained quaternary ammonium salt of triphenyl phosphine carries out Witting reaction with citral in organic solvent II and at the temperature of -20 DEG C-80 DEG C, and 10, 14-dimethyl-7, 9, 13-pentadec-1-triethylenic alcohols is produced; the triethylenic alcohols produced is reduced into 10, 14- dimethyl-1-pentadecanol in organic solvent III through catalysis and hydrogenation; finally, the 10, 14-dimethyl-1-pentadecanol obtained reacts with iso-butyryl chloride in the existence of the organic base II, so that 10, 14-dimethyl pentadec isobutyl is obtained. The invention has the advantages of easily obtained raw material, low cost, moderate reaction, suitability for scale production and high yield.

The present invention relates to a method for preparing 1-ortho-hydroxy phenyl butanone. In the presence of a catalyst of Lewis acid, anisole and butyryl chloride are reacted with an organic solvent as the reaction media at a circumfluence temperature for 2 to 3 hours. The reaction liquid is hydrolyzed by hydrochloric acid. A hydrolysate is separated from the reaction liquid so as to obtain an organic phase. The organic phase is dried by anhydrous magnesium sulfate, and then an organic solvent in the organic phase is removed through reduced pressure distillation so as to obtain 1-ortho-hydroxy phenyl butanone. The removed organic solvent can be recycled. The method is short in process flow, and high in product yield that usually reaches up to more than 90 percent. The obtained 1-ortho-hydroxy phenyl butanone is high in purity that reaches up to more than 95 percent usually. The reaction condition is mild and the three wastes are not discharged.

The invention discloses an Afatinib (I) preparation method which comprises the following steps: performing etherification reaction on 4-chloro-6-amino-7-hydroxyquinazoline (II) and (S)-3-hydroxytetrahydrofuran to generate 4-chloro-6-amino-7-[(S)-(tetrahydrofuran-3-yl)oxy]quinazoline (III); performing acylation reaction on the compound (III) and 4-(N,N-dimethylamino)-2-ene-butyryl chloride to generate 4-chloro-6-{[4-(N,N-dimethylamino)-1-oxo-2-butene-1-yl]amino}-7-[(S)-(tetrahydrofuran-3-yl)oxy]quinazoline (IV); and performing condensation reaction on the compound (IV) and 4-fluoro-3-chloroaniline to obtain Afatinib (I). The preparation method is simple, economic and environment-friendly in process, and meets the requirements for large-scale industrialization.

The invention provides a method for preparing 3,3-dimethyl butyraldehyde, which comprises the following steps of: adding an acid-binding agent, a catalyst, an auxiliary catalyst and a solvent into 3,3-dimethyl butyryl chloride, and reacting under a certain pressure of H2 to obtain the 3,3-dimethyl butyraldehyde, wherein the acid-binding agent is from inorganic base or organic base; the catalyst is selected from recyclable precious metals; and the auxiliary catalyst is a metal salt. The method is suitable for the large-scale industrial production of the 3,3-dimethyl butyraldehyde; in the method, the raw materials used are cheap and readily available, the drawback that a large amount of hydrogen is discharged into the atmosphere in a normal-pressure reaction is overcome; and the method is environmentally-friendly; the reaction is compete, the product yield and product purity are high, the post treatment is simple and the production cost is low.

The invention relates to a method for preparing gamma-tertiary butyl-chlorobenzene butanone. The method is characterized by comprising the following steps of: (1) acylation reaction: sucking butyrolactone into a clean and dry reaction kettle and strring, and then adding zinc chloride into the reaction kettle for reaction to generate semi-finished butyl chloride; (b) hydrolysis reaction: adding dichloroethane and aluminium choride into a clean and dry reaction kettle, dropwise adding the butyl chloride into the reaction kettle while stirring; then continuing to dropwise adding tedin benzene , and steaming off dichloroethane to generate the gamma-tertiary butyl-chlorobenzene butanone. 3gamma-tertiary butyl-chlorobenzene butanone products prepared by the method are pale yellow granules, wherein the content of the 3gamma-tertiary butyl-chlorobenzene butanone is more than or equal to 90 percent, and the pH value is larger than or equal to 3.85. The reaction process of the method is easy to control, the utilization rate of raw materials and the yield of the products are improved, and the method conforms to the requirements on environmental protection and cleaner production and improves the economic benefits of enterprises.

The invention discloses a synthesis method of spirodiclofen which uses 1-cyano cyclohexanol, 2, 4-dichlorobenzene acetyl chloride and 2, 2-dimethyl butyryl chloride as main raw materials. The synthesis method comprises (1) generating a compound II as 2, 4-dichlorobenzene acetic acid-1-cyano cyclohexyl, (2) generating a compound III as 1-[2-(2, 4-dichloro-phenyl)-acetoxy]-cyclohexane methyl formate, (3) generating a compound IV as 3-(2, 4-dichlorophenyl)-2-oxo-1-oxaspiro [4. 5]-sebacic-3-ene 4-alcohol, (4), generating a compound I as 3-(2, 4-dichlorophenyl)-2-oxo-1-oxaspiro [4. 5]-sebacic-3-ene4-radical-2, 2-dimethyl butyl. The spirodiclofen synthesis method has high yield and is suitable for industrial production.

The invention provides a synthesis method of a budesonide impurity USP-Z1. According to the synthesis method, firstly, budesonide is taken as a raw material and subjected to a reaction with butyryl chloride or butyric anhydride under the condition of an organic solvent and an acid-binding agent to produce a compound USP-Z1-IM1; then, the compound USP-Z1-IM1 is dissolved in the organic solvent, anoxidant is added, oxidation is performed, and the impurity USP-Z1 is produced. The synthesis method adopts a simple process route and is convenient to operate, good in selectivity and high in yield; the synthesized budesonide impurity USP-Z1 can serve as a reference substance for detection and study of budesonide and is applied to quality control of budesonide and related preparations to control the purity of raw materials or preparations of budesonide.