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Preparation method of cefminox sodium powder-needle preparation for injection

A technology for sporminol sodium powder and injection, which is applied in the field of biomedical synthesis, can solve the problems of long production process route, complicated steps, and low utilization rate of raw materials, and achieve good product quality, high utilization rate of raw materials, and low cost Effect

Inactive Publication Date: 2017-04-19
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cefminox sodium is a mycin derivative, which is mainly prepared by semi-synthetic method at present. In the prior art, the production process route of cefminox sodium is long, the steps are complicated, and the utilization rate of raw materials is not high

Method used

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preparation example Construction

[0022] The invention discloses a preparation method of cefminox sodium powder preparation for injection, which comprises the following process steps:

[0023] a. Raw material preparation: Mix and stir 2-picoline and dichloromethane until clarified for later use, add bromoacetyl bromide to -35° dichloromethane and keep warm and stir evenly for later use, take cefminox sodium intermediate 7-AMCA spare;

[0024] b. Feed for acylation reaction: add 7-AMCA and dichloromethane into a dry reaction vessel, drop the temperature of the system to -20°C and add 2-picoline solution and bromoacetyl bromide solution dropwise at the same time, and finish adding within 1.5 hours. Then heat up to -15°C and keep the temperature until the end of the reaction;

[0025] c. Decarboxylation protection reaction: add trimethylchlorosilane and anisole, cool down to -40°C, and pass in dried hydrogen chloride gas for 3 hours until the end of the reaction to obtain a reaction solution;

[0026] d. Raise...

Embodiment 1

[0034] The preparation method of injection cefminox sodium powder injection in the present embodiment comprises the following process steps:

[0035] a. Preparation of raw materials: Mix and stir 9g of 2-picoline and 100ml of dichloromethane until clarified for later use, add 20g of bromoacetyl bromide into 100ml of dichloromethane at a temperature of -35°, keep warm and stir evenly for later use, take cefminox Sodium 50g intermediate 7-AMCA for later use.

[0036] b. Add raw materials for acylation reaction: Add 50g of 7-AMCA and 500ml of dichloromethane into a dry 1000ml reaction vessel, drop the temperature of the system to -20°C and add the 2-picoline solution and bromine prepared in step a at the same time Acetyl bromide solution was added in 1.5 hours, then the temperature was raised to -15°C, and the temperature was kept until the end of the reaction;

[0037] c. Decarboxylation protection reaction: add trimethylchlorosilane and anisole, cool down to -40°C, and pass th...

Embodiment 2

[0041] The preparation method of injection cefminox sodium powder injection in the present embodiment comprises the following process steps:

[0042] a. Preparation of raw materials: Mix and stir 15g of 2-picoline and 166.67ml of dichloromethane until clarified for later use, add 20g of bromoacetyl bromide into 166.67ml of dichloromethane at a temperature of -35°, keep warm and stir evenly for later use, take cephalosporin Minol sodium 83.33g intermediate 7-AMCA for later use.

[0043] b. Add raw materials for acylation reaction: Add 50g of 7-AMCA and 833.33ml of dichloromethane into a dry 1000ml reaction vessel, drop the temperature of the system to -20°C and add the 2-picoline solution prepared in step a and The bromoacetyl bromide solution was added in 1.5 hours, then the temperature was raised to -15°C, and the temperature was kept until the end of the reaction;

[0044] c. Decarboxylation protection reaction: add trimethylchlorosilane and anisole, cool down to -40°C, and...

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Abstract

The invention discloses a preparation method of a cefminox sodium powder-needle preparation for injection, and belongs to the technical field of biomedical synthesis. The method comprises: mixing the prepared raw materials, respectively carrying out an acylation reaction and a carboxyl protection removing reaction, treating the solution obtained after the reaction to obtain cefminox, adding sodium carbonate, and crystallizing to obtain cefminox sodium. According to the present invention, the steps are simple, the ladder temperature control mode is used in the reaction temperature control, the complete reaction is ensured through the material feeding time limiting while the production efficiency is improved, the quality of the prepared product is good, and the raw material utilization rate is high.

Description

technical field [0001] The invention relates to a preparation method of cefminox sodium powder preparation for injection, which belongs to the technical field of biomedicine synthesis. Background technique [0002] The "Major New Drug Creation" project is a large-scale scientific and technological development plan in my country. Through the implementation of this special project, my country will accelerate the research and development of a number of new drugs with independent intellectual property rights and market competitiveness, and establish a number of internationally advanced technologies. A platform to form a new drug innovation capability and technology system that supports the independent development of my country's pharmaceutical industry. According to the requirements of the national guidelines for "Major New Drug Creation and Technology Major Projects", relying on the national super-large pharmaceutical industry enterprise North China Pharmaceutical Group Co., Ltd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K9/14C07D501/57C07D501/04C07D501/12A61K31/546A61P31/04
CPCA61K9/14A61K9/0019A61K31/546C07D501/04C07D501/12C07D501/57
Inventor 杨梦德蒋晓声张锁庆张文胜刘萍王智马亚微孙玉双徐薇薇杨轩
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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