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82 results about "Glycine methyl ester" patented technology

Improved method for preparing amoxicillin by enzymic method

The invention relates to the field of pharmacy, and provides an improved method for preparing amoxicillin by an enzymic method, and a product obtained by the improved method for preparing amoxicillin by the enzymic method. The method comprises the following steps of: 1) dissolving 6-aminopenicillanic acid (6-APA) at the temperature of between 10 and 20 DEG C by using water or/and aqueous solution of ammonia which has the pH value of 7.0 to 8.0, and adding D-p-Hydroxyphenylglycine methyl ester hydrochlorid and penicillin G acyltransferase; 2) adjusting the pH value of a solution obtained in the step 1) to be 6.0 to 6.5, and reacting at the temperature of between 21 and 30 DEG C until the content of 6-APA is less than 5mg/ml to obtain a solution of an amoxicillin product; and 3) separating the penicillin G acyltransferase from the solution of the amoxicillin product, adjusting by using hydrochloric acid until the solution of the amoxicillin product is clarified, adding the aqueous solution of ammonia, adjusting the pH value to be 5.5 to 6.5, and crystallizing at the temperature of between 0 and 5 DEG C to obtain amoxicillin. By the improved method for preparing amoxicillin by the enzymic method, the quality of the amoxicillin product is greatly improved, and the medication safety of the amoxicillin product is further improved.
Owner:UNITED LAB INNER MONGOLIA CO LTD

Method for comprehensively recovering effective ingredients in amoxicillin mother liquid prepared by enzyme process

The invention relates to a method for comprehensively recovering effective ingredients in amoxicillin mother liquid prepared by an enzyme process. The method comprises the following steps: (1) concentrating the amoxicillin mother liquid, namely adjusting the pH value of the amoxicillin mother liquid prepared by the enzyme process to be 8.0-9.5, and performing nanofiltration and concentration to obtain concentrated mother liquid; (2) synthesizing amoxicillin under enzyme catalysis, namely adjusting the pH value of the concentrated mother liquid to be 5.8-7.0, and converting 6-APA (6-amino penicillanic acid) and D-methyl hydroxyphenyl glycinate into amoxicillin in the presence of immobilized penicillin acylase for synthesis; (3) preparing D-hydroxyphenyl glycine concentrated liquid by ultrafiltration and nanofiltration, namely separating after the enzyme catalysis reaction is ended to obtain amoxicillin crystals and secondary amoxicillin mother liquid, and performing ultrafiltration and nanofiltration on the secondary mother liquid to obtain the D-hydroxyphenyl glycine concentrated liquid; (4) crystallizing D-hydroxyphenyl glycine. According to the method, 6-APA and D-methyl hydroxyphenyl glycinate remained in the mother liquid are consumed through an indirect process of synthesizing amoxicillin under enzyme catalysis, the product quality of D-hydroxyphenyl glycine is improved, and the yield of D-hydroxyphenyl glycine is increased.
Owner:SHANXI WEIQIDA PHARMA IND

Preparation method of D-para hydroxybenzene glycine methyl ester

The invention provides a preparation method of D-para hydroxybenzene glycine methyl ester. The method comprises the following steps of: firstly, preparing a hydrochloric acid methanol solution; adding D-para hydroxybenzene glycine into the hydrochloric acid methanol solution to perform reflux reaction for 2-4 hours at 65-80 DEG C; performing pressure reduction distillation and removing methanol; and adding water to obtain a D-para hydroxybenzene glycine methyl ester aqueous solution. Based on that, the invention also provides anenzymatic synthesis method of amoxicillin. The method comprises the following steps of: adding 6-APA and immobilized penicillin acylase into the D-para hydroxybenzene glycine methyl ester aqueous solution to react for 1-8 hours at 10-30 DEG C; regulating the pH value of a reaction liquid to 0.8-1.0 by using hydrochloric acid or sulfuric acid aqueous solution; regulating the pH value to 4.5-6.0 by using ammonia water or sodium hydroxide aqueous solution to crystallize for 1-5 hours at 0-30 DEG C; separating solid from liquid; collecting a solid; and washing and drying to obtain amoxicillin. The method is simple in steps, and low in cost; and the obtained -para hydroxybenzene glycine methyl ester is high in yield and less in impurities and can be directly applied to anenzymatic synthesis of amoxicillin.
Owner:NORTH CHINA PHARM GRP SEMISYNTECH CO LTD

Process for direct preparation of amoxicillin by liquid 6-APA (amino penicillanic acid)

The invention belongs to the technical field of medicine preparation and relates to a process for direct preparation of amoxicillin by liquid 6-APA (amino penicillanic acid). The process includes: taking penicillin degreasing solution as an initial material, sequentially performing cracking reaction, extraction, phase splitting, resin column adsorptive purification, distillation and concentration to obtain a 6-APA solution with the concentration being 80-100g/L, and synthesizing with p-hydroxyphenylglycine methyl ester under a catalytic action of type-II penicillin G acylase to obtain the amoxicillin. Compared with a traditional method, the process has the advantages that subsequent steps of 6-APA crystallization, centrifuging, drying and the like are avoided, investment of fixed assets is reduced, energy loss, equipment loss and cost are reduced, profits are increased, and physical injuries of staffs are reduced. Compared with existing direct amoxicillin preparation methods, the process has the advantages that by adoption of dichloromethane as an extracting agent, total mole yield of amoxicillin is higher relatively, the extracting agent is easy for distillation separation, the content of residual solvents in products is greatly reduced, medication safety is improved, and the process is worthy of popularization in production.
Owner:INNER MONGOLIA CHANGSHENG PHARMA

Aromatic substitution spiro indolyl diketopiperazine compound and synthesis method thereof

The invention discloses an aromatic substitution spiro indolyl diketopiperazine compound and a synthesis method thereof. Glycine is used as a raw material and subjected to esterification reaction with methyl alcohol and thionyl chloride to obtain methyl glycinate hydrochloride, methyl glycinate hydrochloride and aromatic aldehyde are subjected to condensation reaction to obtain Schiff base, isatin is used as a raw material and subjected to reduction reaction under the action of hydrazine hydrate to obtain indoline-2-ketone, indoline-2-ketone and benzaldehyde are subjected to Knoevenagel reaction under piperidine catalysis to obtain 3-phenylidene-1,3-dihydro-2H-indol-2 ketone, 3-phenylidene-1,3-dihydro-2H-indol-2 ketone and Schiff base are subjected to 1,3-dipole cycloaddition reaction under catalysis of chiral ligand (S)-TF-BiphamPhos/AgoAc to obtain spiro pyrrolidine, and protecting group removal and ring closure are carried out on spiro pyrrolidine and N-(9-fluorene methoxycarbonyl)-L-prolyl chloride through base catalysis to obtain the target product. The method has the advantages of being simple in path, high in yield, high in diastereoselectivity and single in product spatial configuration, and the raw materials are low in price and easy to obtain.
Owner:SHAANXI UNIV OF SCI & TECH

Method for synthesizing D-p-hydroxyphenylglycine methyl ester

The invention relates to the field of compound synthesis and discloses a method for synthesizing D-p-hydroxyphenylglycine methyl ester. The method comprises steps as follows: (1), in the presence of thionyl chloride, D-p-hydroxyphenylglycine resolving agent salt and methanol have an esterification reaction, and D-p-hydroxyphenylglycine methyl ester resolving agent salt is obtained; (2), the D-p-hydroxyphenylglycine methyl ester resolving agent salt and alkaline metal hydroxide are dropwise added to a D-p-hydroxyphenylglycine methyl ester aqueous solution at the temperature of 10-15 DEG C, the pH (potential of hydrogen) value of a system is controlled in the range from 6.5 to 7 in the dropwise adding process, after dropwise adding of the D-p-hydroxyphenylglycine methyl ester resolving agent salt is completed, alkaline metal hydroxide is continuously dropwise added until the pH value of the system ranges from 7.5 to 8, a crystal is grown at the temperature of 10-15 DEG C and under the condition of the pH value being 7.5-8, an obtained crystalline liquid is filtered, and a D-p-hydroxyphenylglycine methyl ester crystal and a mother liquor are obtained. With adoption of the method provided by the invention, D-p-hydroxyphenylglycine methyl ester with a higher yield can be produced.
Owner:山西双雁生物科技有限公司
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