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Synthesis method for cefminox sodium

A technology of cefminox sodium and a synthesis method, which is applied to the synthesis field of cefminox sodium, can solve the problems of long reaction route and many unit operations, and achieves the effects of short process route, low price and low cost

Active Publication Date: 2014-09-10
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 reaction route is long and there are many unit operations

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A kind of synthetic method of cefminox sodium is provided, comprising the steps of:

[0018] (1) Add 50g of cefminox core 7-AMCA and 500mL of dichloromethane into a dry 1000mL reaction flask, add 9g of 2-picoline after the system cools down to -15±2°C, add dropwise 20g of bromoacetyl bromide to keep React for 1 hour;

[0019] (2) After the reaction is complete, add trimethylchlorosilane and anisole, cool down to -40°C, and then feed metered hydrogen chloride gas for 3 hours, and the reaction ends;

[0020] (3) Warm up to 3±2°C, add Na dropwise 2 CO 3 Saturated solution, control the pH value to 6.5±0.2, separate layers, transfer the water phase to another 1000ml three-necked bottle, add 500ml ethyl acetate, dropwise add hydrochloric acid solution with a mass fraction of 15%, adjust the pH value to 0.5, stir, Stand for stratification, separate ethyl acetate, add dropwise 15g of D-cysteine ​​hydrochloride aqueous solution to ethyl acetate, dropwise add triethylamine, co...

Embodiment 2

[0023] A kind of synthetic method of cefminox sodium is provided, comprising the steps of:

[0024] (1) Add 50g of 7-AMCA and 800mL of dichloromethane into a dry 1000mL reaction flask, cool down to -20±2°C, add 14g of N,N-xylidine, dropwise add 20g of bromoacetyl bromide, and maintain this temperature for reaction 1.5 hours;

[0025] (2) After the reaction is completed, trimethyliodosilane and anisole are added, the temperature is lowered to -35°C, and metered hydrogen chloride gas is introduced for 2 hours;

[0026] (3) Heat up to 0~5℃ and add K dropwise 2 CO 3 Solution, control the pH value to 7.0±0.2, separate layers, transfer the water phase to another 1000mL three-necked bottle, add 1000mL ethyl acetate, dropwise add hydrochloric acid solution with a mass fraction of 15%, adjust the pH value to 0.8, stir, and statically Separate the layers, separate the ethyl acetate, add dropwise 14.5g D-cysteine ​​hydrochloride aqueous solution to the ethyl acetate solution, add diet...

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Abstract

The invention discloses a synthesis method for cefminox sodium. The method comprises the following steps: by taking cefminox mother nucleus 7-AMCA as a raw material, carrying out acylation reaction and decarboxylate protection reaction to obtain a mixed liquor; processing and condensing the mixed liquid into cefminox acid, and salifying without separation of an intermediate to synthesize cefminox sodium in one step. In the manner, by adopting the synthesis method for cefminox sodium disclosed by the invention, a plurality of reaction steps can be finished one time without separation, a sterile cefminox sodium product can be obtained by a continuous operation one time, the total yield can be up to 90% by taking 7-AMCA as an initial raw material, the process route is short, and the adopted reaction agent is low in price and low in cost.

Description

technical field [0001] The invention relates to the technical synthesis field of biomedicine and chemical engineering, in particular to a synthesis method of cefminox sodium. Background technique [0002] Cefminox sodium is a third-generation broad-spectrum cephalosporin antibiotic, which was launched by Japan's Meiji Pharmaceutical in 1987. The English name of cefminox sodium is Cefminox Sodium, and the chemical name is (6R,7S)-7-[(S)-2-(2-amino-2-carboxyethylmercapto)acetamido]-7-methoxy- 3-[[(1-methyl-1H-5-yl)thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2 - Sodium carboxylate, generally in the form of heptahydrate crystals, with the molecular formula C 16 h 20 N 7 NaO 7 S 3 ·7H 2 O, the molecular weight is 667.67, and the structural formula is: [0003] . [0004] The earliest synthetic route of cefminox sodium is relatively long, with 7-ACA as the starting material, after carboxyl protection, 3-position side chain connection, 7-position methoxy subst...

Claims

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Application Information

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IPC IPC(8): C07D501/57C07D501/04
CPCC07D501/04C07D501/57
Inventor 周自金黄军豪张群芳陈雷温雄飞罗新祖
Owner 苏州盛达药业有限公司
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