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A kind of preparation method of cefazolin sodium impurity b

A technology of cefazolin sodium and cefazolin, which is applied in the field of preparation of cefazolin sodium impurity B, can solve problems such as antibiotic allergy, drug quality decline, life-threatening, etc., and achieves mild reaction conditions, high yield, and reduced process The effect of steps

Active Publication Date: 2022-05-10
PI & PI BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to different processes, the sources of related substances of cephalosporins are different, and there are side reactions introduced during the synthesis process, starting materials and intermediates, degradation, etc., which will cause the quality of the drug to decline. At the same time, such impurities will cause reactions such as antibiotic allergies. , even life-threatening

Method used

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  • A kind of preparation method of cefazolin sodium impurity b
  • A kind of preparation method of cefazolin sodium impurity b
  • A kind of preparation method of cefazolin sodium impurity b

Examples

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Effect test

Embodiment 1

[0025] The preparation method of cefazolin sodium impurity B described in the present embodiment comprises the following steps:

[0026] Weigh 1 g of cefazolin core, dissolve it in 40 mL of tetrahydrofuran, add 2 drops of pyridine dropwise, cool down to 0 °C, add 0.5 mL of pivaloyl chloride dropwise, and react at room temperature for 2.5 hours. After the reaction is complete, add 150 mL of water to precipitate crystals, filter , the crystals were added with 50 mL of water and beaten for 2.5 hours, filtered and dried to obtain cefazolin sodium impurity B with a purity of 95%, and a yield of 65.2%.

Embodiment 2

[0028] The preparation method of cefazolin sodium impurity B described in the present embodiment comprises the following steps:

[0029] Weigh 1 g of cefazolin core, dissolve it in 30 mL of tetrahydrofuran, add 2 drops of pyridine dropwise, cool down to 0 °C, add 0.5 mL of pivaloyl chloride dropwise, and react at room temperature for 2 hours. After the reaction is complete, add 100 mL of water to precipitate crystals, filter, Add 50 mL of water to the crystals, beat for 2.5 hours, filter and dry to obtain cefazolin sodium impurity B with a purity of 95%, and a yield of 55.3%.

Embodiment 3

[0031] The preparation method of cefazolin sodium impurity B described in the present embodiment comprises the following steps:

[0032] Weigh 1 g of cefazolin mother nucleus, dissolve it in 20 mL of tetrahydrofuran, add 1 drop of pyridine dropwise, cool down to 0 °C, add 0.35 mL of pivaloyl chloride dropwise, and react at room temperature for 2 hours. After the reaction is complete, add 100 mL of water to precipitate crystals, filter, Add 100 mL of water to the crystals, beat for 2 hours, filter and dry to obtain cefazolin sodium impurity B with a purity of 95%, and a yield of 51.5%.

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Abstract

The invention discloses a preparation method of cefazolin sodium impurity B. The invention uses the cefazolin mother nucleus as a raw material, undergoes acylation reaction with pivaloyl chloride, crystallizes and beats, filters and dries to obtain the cefazolin sodium impurity B. The invention has mild reaction conditions, does not involve ultra-low temperature reaction, reduces process steps, and is suitable for laboratory scale-up. The cefazolin sodium impurity B prepared according to the method of the invention has a high yield and a purity of 95%, can meet the quality research requirements of the cefazolin sodium, and provides a technical basis for improving the national quality standard of the cefazolin sodium.

Description

technical field [0001] The invention relates to the field of pharmaceutical impurities, in particular to a preparation method of cefazolin sodium impurity B. Background technique [0002] Cefazolin sodium (Cefazolin sodium), also known as Pioneer V, is the strongest of the first-generation cephalosporins. Ideal and other advantages, it has good antibacterial activity against other Gram-positive cocci, and is a semi-synthetic cephalosporin commonly used in clinical practice. Due to the production process and structural characteristics of antibiotics, the research on related substances (impurities) is an important and difficult point in drug quality control. Due to different processes, the sources of related substances of cephalosporins are different, and there are side reactions introduced during the synthesis process, starting materials and intermediates, degradation, etc., which will cause the quality of the drug to decline. At the same time, such impurities will cause rea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/36C07D501/06
CPCC07D501/36C07D501/06
Inventor 袁晓林顺权
Owner PI & PI BIOTECH