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A kind of preparation method of cefazolin sodium impurity g

A technology for cefazolin sodium and acetyl cefazolin is applied in the field of preparation of cefazolin sodium impurity G, can solve the problems of antibiotic allergy, drug quality decline, life-threatening and the like, and achieves the effects of simple process steps and mild reaction conditions

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

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

Examples

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Embodiment 1

[0030] The preparation method of cefazolin sodium impurity G described in the present embodiment comprises the following steps:

[0031] (1) At room temperature, weigh 2 g of cefazolin sodium impurity D, add 100 mL of water, add sodium bicarbonate to adjust the pH to 8.5, heat in an oil bath at 50° C. for 4 hours to carry out the hydrolysis reaction, and obtain a reaction solution containing deacetylated cefazolin;

[0032] (2) Add 3mol / L hydrochloric acid to the reaction solution containing deacetylated cefazolin to adjust the pH to 2, carry out the ring closure reaction for 3 hours, and obtain the reaction solution containing cefazolin sodium impurity G, and the reaction solution containing cefazolin sodium impurity G Separation and purification on a 70mL C18 column, eluting with 300mL of 0.05% formic acid water, 1% acetonitrile acid water, and 3% acetonitrile acid water respectively, diluting the pure fraction by 2 times, loading the sample on a 70mL PIPI-02 column, eluting ...

Embodiment 2

[0034] The preparation method of cefazolin sodium impurity G described in the present embodiment comprises the following steps:

[0035] (1) At room temperature, weigh 2 g of cefazolin sodium impurity D, add 100 mL of water, add sodium bicarbonate to adjust the pH to 9, and heat in an oil bath at 50°C for 4 hours to react to obtain a reaction solution containing deacetylated cefazolin;

[0036] (2) Add 4mol / L hydrochloric acid to the reaction solution containing deacetylated cefazolin to adjust the pH to 1, carry out the ring closure reaction for 3 hours, and obtain the reaction solution containing cefazolin sodium impurity G, and the reaction solution containing cefazolin sodium impurity G Separation and purification on a 70mL C18 column, eluting with 300mL of 0.05% formic acid water, 1% acetonitrile water and 3% acetonitrile water respectively. The pure fraction was diluted 2 times, loaded on a 70mL PIPI-02 column, eluted with 80% acetonitrile, and freeze-dried to obtain cef...

Embodiment 3

[0038] The preparation method of cefazolin sodium impurity G described in the present embodiment comprises the following steps:

[0039] (1) At room temperature, weigh 2 g of cefazolin sodium impurity D, add 160 mL of water, add sodium bicarbonate to adjust the pH to 9, and heat in an oil bath at 50°C for 3 hours to react to obtain a reaction solution containing deacetylated cefazolin;

[0040] (2) Add 4mol / L hydrochloric acid to the reaction solution containing deacetylated cefazolin to adjust the pH to 1, carry out the ring closure reaction for 2.5h, and obtain the reaction solution containing cefazolin sodium impurity G, and the reaction solution containing cefazolin sodium impurity G Separation and purification on a 70mL C18 column, eluting with 300mL of 0.05% formic acid water, 1% acetonitrile water, and 3% acetonitrile water respectively. The pure fraction was diluted 2 times, loaded on a 70mL PIPI-02 column, eluted with 80% acetonitrile, and freeze-dried to obtain cefaz...

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Abstract

The invention discloses a preparation method of cefazolin sodium impurity G. The present invention adopts cefazolin sodium impurity D hydrolysis reaction to obtain deacetyl cefazolin, deacetyl cefazolin undergoes ring closing reaction, obtains cefazolin sodium impurity G through separation and purification, and the reaction conditions are mild in the preparation method, and the process steps are simple , and does not involve ultra-low temperature reactions. The yield of impurity G of cefazolin sodium prepared by the invention is 61.4%-64.8%, and the purity can reach 95%, which can meet the quality research requirements of cefazolin sodium, and provides a technical basis for the improvement of the national quality standard of 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 G. 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): C07D501/04C07D501/12C07D501/00
CPCC07D501/04C07D501/12C07D501/00
Inventor 袁晓林顺权
Owner PI & PI BIOTECH