Method for preparing cefamandole nafate sodium powder injection preparation for injection

A technology for mendolate sodium powder and injection, which is applied in the field of preparation of cefamandole sodium powder for injection, to achieve the effects of quality optimization, improvement of reaction efficiency, and change of crystallization mode

Inactive Publication Date: 2019-10-08
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 sodium powder injection 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 ob...

Embodiment 2

[0053] 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;

[0054] 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;

[0055] 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;

[0056] 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

[0062] 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;

[0063] 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;

[0064] 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;

[0065] 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 sodium powder injection preparation for injection. The method comprises the following steps: (1) dissolution of N,N-dimethylaniline;(2) dissolution of D-formylmandeloyl chloride; (3) silanization reaction; (4) synthesis of cefamandole acid esters; (5) extraction; (6) dehydration and decoloration; (7) crystallization; and (8) sterilized shipment. By changing the modes of charging and crystallization, the reaction efficiency and the product appearance quality are improved.

Description

[0001] This application is a divisional application of the Chinese application submitted on September 30, 2016 with the application number 201610874006.0 and the invention name is "Method for preparing cefamandole sodium powder injection preparation". technical field [0002] 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 [0003] Cefamandole sodium, as a relatively large variety of cephalosporins, currently has a huge market potential. This product is a second-generation cephalosporin antibiotic, and its chemical name is: (6R, 7R)-7(R)-(2-formyloxy-2-phenylacetamido]-3[[(1 -Methyl-1H-tetrazol-5-yl)thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid Sodium salt. Calculated on anhydrous basis, it contains 84.0%-93.0% of cefamandole (C18H17N6NaO6S2). [0004] This product can usually be used for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K31/546C07D501/36C07D501/04A61P31/04A61K9/14
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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