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Method for synthesizing cefmenoxime hydrochloride

A technology for cefmenoxime hydrochloride and hydrochloric acid, which is applied in the field of synthesizing cefmenoxime hydrochloride, can solve problems such as difficult separation and drying, difficult recovery of solvents, poor crystal form, etc., and achieves easy separation and drying, and convenient solvent recovery , low cost effect

Inactive Publication Date: 2015-03-25
苏州盛达药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The conversion rate of the mixed solvent used in the existing literature reports is low, the solvent is not easy to recover, and other separation methods such as adsorption are needed instead of a single recrystallization method. The obtained crystal form is not good, and it is not easy to separate and dry

Method used

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Embodiment 1

[0017] A method for synthesizing Cefmenoxime Hydrochloride is provided, comprising the steps of:

[0018] (1) Using 7-ACA as the starting material, the intermediate 7-ATCA or 7-ATCA hydrochloride was obtained through condensation of 7-ACA and 1-methyl-5-mercapto-1H-tetrazolium. in

[0019] (2) In a dry 500ml three-necked flask, add 40g 7-ATCA, 300ml dichloromethane and 46g AE active ester, and cool down to 5°C. Add 20g of triethylamine dropwise and stir the reaction. After 5 hours, take a sample to measure the reaction end point. After the end point is qualified, add 160ml of water for multiple extractions, combine the water phase, add 4g of activated carbon to the water phase, stir and decolorize at 20°C to 22°C for 1h, filter and wash with water carbon. Add 600ml of acetone, add hydrochloric acid solution to adjust the pH value to 2.4-2.6, add seed crystals, stir and grow crystals for 4 hours, filter and wash with water and acetone. Dry at 40°C to 45°C until the moisture ...

Embodiment 2

[0023] A method for synthesizing Cefmenoxime Hydrochloride is provided, comprising the steps of:

[0024] (1) Using 7-ACA as the starting material, the intermediate 7-ATCA or 7-ATCA hydrochloride is obtained through condensation of 7-ACA and 1-methyl-5-mercapto-1H-tetrazolium;

[0025] (2) Add 40g of 7-ATCA hydrochloride, 250ml of dichloromethane and 45g of AE active ester into a dry 500ml three-neck flask, add 20g of diethylamine dropwise, control the temperature at 0℃~5℃, stir the reaction, and take a sample after 3h Measure the reaction end point, after the end point is qualified, add 150ml of water for multiple extractions, combine the water phase, add 4g of activated carbon to the water phase, stir and decolorize at 20°C-22°C for 1h, filter, and wash the carbon with water. Add 600ml of ethanol to the water phase, add dropwise 2mol / L hydrochloric acid solution to adjust the pH to 2.2-2.4, add seed crystals, stir and grow crystals for 4 hours, filter and wash with water and...

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Abstract

The invention discloses a method for synthesizing cefmenoxime hydrochloride. The method comprises the following steps: dissolving 7-ATCA or 7-ATCA hydrochloride and AE-active ester in dichloromethane, and dropwise adding organic alkali at -5-15 DEG C; adding water to extract for multiple times after the reaction is completed, decolorizing the water phase, adding a hydrophilic solvent, and dropwise adding hydrochloric acid at 10-35 DEG C to crystallize and separate cefmenoxime hydrochloride. According to the method for synthesizing cefmenoxime hydrochloride, the condensation system reacts by adopting a single solvent with high conversion rate, and the solvent is convenient to reclaim; the method for synthesizing cefmenoxime hydrochloride is direct crystallization and separation, and adsorption and other separation methods are not needed, so that cefmenoxime hydrochloride has good crystalline form, is easy to separate and dry, simple in synthesizing route and low in cost, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of medicine and chemical industry, in particular to a method for synthesizing cefmenoxime hydrochloride. Background technique [0002] Cefmenoxime hydrochloride belongs to the third generation of broad-spectrum cephalosporin antibiotics, developed by Japan's Takeda Pharmaceutical Industry, and successfully launched in October 1982. In the past, the synthetic process route of cefmenoxime hydrochloride was long and complicated. With the industrialized supply of the key intermediate 1-methyl-5-mercapto-1H-tetrazolium and AE active ester, the synthetic route becomes simple, and generally only two to three steps are required to synthesize cefmenoxime hydrochloride . It is reported in the literature that the condensation of 7-ATCA and AE active ester mostly uses a mixed solvent as the condensation solvent. After the reaction is completed, water is added for extraction and separation, and the water phase is adsor...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/06C07D501/12
CPCC07D501/36C07D501/06C07D501/12
Inventor 周自金贾志强钱志勇孙悦铭陈雷杨虎星
Owner 苏州盛达药业有限公司
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