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Method for preparing cefamandole nafate powder preparation for injection

A technology for sodium montorole powder and injection, which is applied in the field of preparation of cefamandole sodium powder for injection for injection, and achieves the effects of quality optimization, improving reaction efficiency and changing crystallization mode.

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

[0007] In the research process of cefamandole sodium production, the different ways of feeding and crystallization affect the reaction efficiency and the appearance quality of the product. At present, there is a lack of a technical method for improving the reaction efficiency and quality of the product.

Method used

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  • Method for preparing cefamandole nafate powder preparation for injection
  • Method for preparing cefamandole nafate powder preparation for injection

Examples

Experimental program
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Effect test

Embodiment 1

[0044] ①Dissolution of N,N-dimethylaniline: Add 14ml of N,N-dimethylaniline into 25ml of dichloromethane at -10°C, stir well and keep at -10°C for later use;

[0045] ②Dissolution of D-formylmandelic acid chloride: Add 18ml of D-formylmandelic acid chloride to a solution of 25ml of dichloromethane at -10°C, stir well and keep at -10°C for later use;

[0046] ③Silylation reaction: Add 30g of 7-TMCA and 340ml of dichloromethane to a 1000ml reaction bottle and stir evenly. When the system temperature is 12°C, add 20ml of hexamethyldisilamine to the above solution, and return Clarification, the reflux temperature is 40°C, reflux reaction for 1.5h, and the temperature of the system is lowered to -10°C to obtain the reaction solution 1;

[0047]④ Synthesis of cefamandoleate: within 1.2 hours, slowly add dropwise the N, N-dimethylaniline dichloromethane solution in step ① and the D-formylmandelic acid in step ② in the reaction solution 1 Acyl chloride dichloromethane solution to obt...

Embodiment 2

[0052] ①Dissolution of N,N-dimethylaniline: Add 14ml of N,N-dimethylaniline into 25ml of dichloromethane at -10°C, stir well and keep at -12°C for later use;

[0053] ②Dissolution of D-formylmandelic acid chloride: Add 18ml of D-formylmandelic acid chloride to a solution of 25ml of dichloromethane at -10°C, stir well and keep at -13°C for later use;

[0054] ③Silylation reaction: Add 50g of 7-TMCA and 570ml of dichloromethane to a 1000ml reaction bottle and stir evenly. When the system temperature is 15°C, add 40ml of hexamethyldisilamine to the above solution, and return Clarification, the reflux temperature is 41°C, the reflux reaction is 1.7h, and the temperature of the system is lowered to -10°C to obtain the reaction solution 1;

[0055] ④ Synthesis of cefamandoleate: within 1.5 hours, slowly add dropwise the N, N-dimethylaniline dichloromethane solution in step ① and the D-formylmandelic acid in step ② in the reaction solution 1 Acyl chloride dichloromethane solution to...

Embodiment 3

[0060] ①Dissolution of N,N-dimethylaniline: Add 30ml of N,N-dimethylaniline into 54ml of dichloromethane at -15°C, stir well and keep at -15°C for later use;

[0061] ②Dissolution of D-formylmandelic acid chloride: Add 18ml of D-formylmandelic acid chloride to a solution of 49ml of dichloromethane at -10°C, stir well and keep at -15°C for later use;

[0062] ③Silylation reaction: Add 45g of 7-TMCA and 500ml of dichloromethane to a 1500ml reaction bottle and stir evenly. When the system temperature is 17°C, add 30ml of hexamethyldisilamine to the above solution and return to Clarification, the reflux temperature is 42°C, reflux reaction for 2h, and the temperature of the system is lowered to -10°C to obtain the reaction solution 1;

[0063] ④ Synthesis of cefamandoleate: within 1.7 hours, slowly add dropwise the N,N-dimethylaniline dichloromethane solution in step ① and the D-formylmandelic acid in step ② in the reaction solution 1 Acyl chloride dichloromethane solution to obt...

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Abstract

The invention discloses a method for preparing a cefamandole nafate powder preparation for injection, wherein the method comprises the following steps: 1, dissolving N,N-dimethyl aniline; 2, dissolving D-formyl mandelic acid chloride; 3, carrying out a silylation reaction; 4, synthesizing cefamandole acid ester; 5, extracting; 6, carrying out dehydration and decolorization; 7, crystallizing; and 8, carrying out aseptic subpackaging. The reaction efficiency and the appearance quality of the product are improved by changing feeding and crystallization ways.

Description

technical field [0001] The invention relates to a method for preparing cefamandole sodium powder injection preparations for injection, and belongs to the field of powder injection preparations of raw materials. Background technique [0002] With North China Pharmaceutical as the lead unit, the United Nations backbone industry-university-research units in the field of microbial pharmacy, through the integration of scientific research resources, key technology innovation and technology platform construction, innovation of cooperation mechanism, in the national major science and technology project "microbial drug technology innovation alliance and new drug In the "Create Industry-University-Research Alliance", for antibiotics in the field of anti-infection, the product quality and purity are improved through process improvement. Cefamandole sodium, as a relatively large variety of cephalosporins, currently has a huge market potential. This product is a second-generation cephal...

Claims

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Application Information

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IPC IPC(8): A61K31/546C07D501/36A61P31/04A61K9/14
CPCA61K9/0019A61K9/141A61K31/546A61P31/04C07D501/04C07D501/36
Inventor 孙燕胡利敏张锁庆杨梦德李敏杨宏硕马亚松米建伟张致一黄晶李雪元
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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