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Method of preparing cefmenoxime E isomers

A technology for cefmenoxime and isomers, which is applied in the field of preparation of cefmenoxime E isomers, can solve the problems of not being prepared, unable to confirm the structure and the like, and achieve the effect of high purity

Inactive Publication Date: 2015-03-25
GUANGZHOU BAIYUSN TIANXIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In addition, it is also reported in the literature that the structure of cefmenoxime E isomer was deduced by analysis by LC-MS method, but the impurity was not obtained, and the structure confirmation could not be carried out.

Method used

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  • Method of preparing cefmenoxime E isomers
  • Method of preparing cefmenoxime E isomers
  • Method of preparing cefmenoxime E isomers

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Weigh 5.0g of 7-ATCA·HCl and 5.77g of trans-AE active ester into a three-necked flask, add 20ml of DMF, 20ml of THF, and 5ml of purified water. While stirring, 4.8ml of triethylamine was added dropwise until the solution was dissolved. After reacting for 2 hours, add 50ml of water and 30ml of dichloromethane to extract, separate the liquid to take the water phase, add 0.2g of activated carbon, stir for 15min, filter, cool the filtrate to below 15°C, add concentrated hydrochloric acid dropwise to pH2.5~3.0, continue stirring for 1h After filtering, the filter cake was vacuum-dried at 35°C to obtain the E isomer of cefmenoxime.

[0023] The purity was 98% by HPLC.

Embodiment 2

[0025] Weigh 5.0g of 7-ATCA·HCl and 5.30g of trans-AE active ester into a three-necked flask, add 20ml of DMF, 25ml of THF, and 5ml of purified water. While stirring, add 2.8ml of concentrated ammonia water dropwise until the solution is dissolved. After reacting for 1 hour, add 50ml of water and 30ml of dichloromethane for extraction, separate the liquid to take the water phase, add 0.2g of activated carbon, stir for 15 minutes, filter, cool the filtrate to below 15°C, add concentrated hydrochloric acid dropwise to pH 2.5-3.0, and continue stirring for 1 hour After filtering, the filter cake was vacuum-dried at 35°C to obtain the E isomer of cefmenoxime.

[0026] The purity was 98% by HPLC.

Embodiment 3

[0028] Weigh 5.0g of 7-ATCA·HCl and 6.25g of trans-AE active ester into a three-necked flask, add 25ml of DMF, 25ml of THF, and 5ml of purified water. While stirring, 1.5 g of sodium hydroxide was added until the solution was dissolved. After reacting for 3 hours, add 50ml of water and 30ml of dichloromethane to extract, separate the liquid to take the water phase, add 0.1g of activated carbon, stir for 15min, filter, cool the filtrate to below 15°C, add concentrated hydrochloric acid dropwise to pH2.0~3.0, continue stirring for 1h After filtering, the filter cake was vacuum-dried at 35°C to obtain the E isomer of cefmenoxime.

[0029] The purity was 97% by HPLC.

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Abstract

The invention relates to a method of preparing cefmenoxime E isomers and is applicable to the need of pharmaceutical enterprises. The method comprises the steps: step (1), suspending 3-[[(1-methyl-1H-tetrazole-5-yl) sulfur] methyl]-7-amino-carboxylate hydrochloride dehydrate (7-ATCA.HCl) and trans AE active ester in a mixed system of water and organic solvent, adding alkaline, stirring and reacting to generate the cefmenoxime E isomers, in which the molar rate of the 3-[[(1-methyl-1H-tetrazole-5-yl) sulfur] methyl]-7-amino-carboxylate hydrochloride dehydrate, the trans AE active ester and the alkaline is 1: 1.1-1.3: 2.5-2.8, and the reaction time is 1-3 hours; step (2) after the reaction is finished, passivating, regulating the pH value to be 2.0-3.0, crystallizing, filtering and drying in vacuum. The prepared cefmenoxime E isomers have high purity which is not less than 97%, and can be used as reference substances for quality control of cefmenoxime hydrochloride bulk drug and preparations thereof.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a preparation method of cefmenoxime E isomer. technical background [0002] Drug impurity research has two important meanings. First, impurity research is necessary to ensure product safety. Secondly, impurity research involves the whole process of pharmaceutical research. The sources of impurities, detection methods, limits, and potential safety hazards of drugs. These factors brought about by impurities have a greater impact on the selection of dosage forms, prescription composition, process determination, research on analytical methods, and product storage. influences. Therefore, impurity research is the focus of drug quality research, quality control and safety research. [0003] Impurity reference substances are an important key to drug impurity research, but the impurities of most drugs are not provided with reference substances, that is, the acquisition of impurity refer...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/04
CPCC07D501/04C07D501/36
Inventor 谭胜连司徒小燕文青闵翠娥江少仪郭泽彬贾永兵
Owner GUANGZHOU BAIYUSN TIANXIN PHARMA
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