New preparation method of ceftiofur sodium

A technology of ceftiofur sodium and ceftiofur sodium, which is applied in the field of preparation of ceftiofur sodium, can solve the problems of reduced production cost, low product yield, low purity, etc., achieves reduced production cost, simple operation, and improved reaction yield. rate effect

Inactive Publication Date: 2011-06-15
SHANGHAI ECUST BIOMEDICINE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In order to better carry out large-scale industrial production of ceftiofur sodium, the preparation method provided by the invention solves the problems of low product yield, easy deterioration, and low purity; selecting a suitable alkali and selecting a suitable solvent improves the reaction yield , while greatly reducing production costs

Method used

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  • New preparation method of ceftiofur sodium
  • New preparation method of ceftiofur sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 2.00g of ceftiofur hydrochloride and 30ml of ethylene glycol monomethyl ether into a 50ml single-necked bottle, stir until completely dissolved, accurately weigh 1.00g of sodium bicarbonate, add it to the system, stir and react until no gas is released, Suction filtration under reduced pressure, pour the filtrate into 400ml tetrahydrofuran, stir for 2 hours until the crystallization is complete, suction filtration, wash the filter cake with acetone, and vacuum dry at room temperature until no more weight loss. 1.73 g of off-white solid was obtained. (The HPLC area normalization method shows that the purity is greater than 98.0%, the HPLC external standard method determines the content is greater than 95.0%, and other indicators of the product meet the quality standards of the Ministry of Agriculture)

Embodiment 2

[0030] Add 2.00g of ceftiofur hydrochloride and 30ml of ethylene glycol monoethyl ether into a 50ml single-necked bottle, stir until completely dissolved, accurately weigh 0.60g of sodium carbonate, add it to the system, stir and react until no gas is released, and decompress Suction filtration, pour the filtrate into 400ml of acetone, stir for 2 hours until the crystallization is complete, suction filtration, wash the filter cake with acetone, and vacuum dry at room temperature until no more weight loss. 1.69 g of off-white solid was obtained. (The HPLC area normalization method shows that the purity is greater than 98.0%, the HPLC external standard method determines the content is greater than 95.0%, and other indicators of the product meet the quality standards of the Ministry of Agriculture)

Embodiment 3

[0032] Add 2.00g of ceftiofur hydrochloride and 30ml of dimethylformamide into a 50ml single-necked bottle, stir until completely dissolved, accurately weigh 1.80g of sodium 2-ethylhexanoate, add it to the system, stir for 2 hours, and depressurize Suction filtration, pour the filtrate into 400ml of ethanol, stir for 2 hours until the crystallization is complete, suction filtration, wash the filter cake with acetone, and vacuum dry at room temperature until no more weight loss. 1.72 g of off-white solid was obtained. (The HPLC area normalization method shows that the purity is greater than 98.0%, the HPLC external standard method determines the content is greater than 95.0%, and other indicators of the product meet the quality standards of the Ministry of Agriculture)

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Abstract

The invention provides a new method for preparing sodium salt from ceftiofur hydrochloride. The method comprises the following step of reacting inorganic weak base such as sodium bicarbonate and the like or organic weak acid with the ceftiofur hydrochloride by using a proper solvent to obtain the sodium salt with high yield. The quality of products reaches quality standard of the Ministry of agriculture. Compared with the conventional process route, the process route has the characteristics of cheap and readily-available selected raw materials and reagents, low process cost, environmental friendliness, high product yield (about 90 percent) and the like and is suitable for industrialized production.

Description

technical field [0001] The invention mainly relates to a preparation method of ceftiofur sodium. Background technique [0002] Since the advent of cephalosporin antibiotics, after more than 60 years of research and development, more than 60 varieties of antibiotics have been developed into 4 generations, which have greatly improved human living standards and quality of life. However, in recent years, the abuse of antibiotics, especially the abuse of antibiotics shared by humans and animals, has caused many bacteria to develop resistance to antibiotics. People have to increase the dosage of antibiotics, and are also forced to study new antibiotics to combat the existing resistance. Medicinal bacteria. While investing a lot of money, it also increases the environmental burden, so the problem of antibiotic abuse is becoming more and more serious. The abuse of antibiotics shared by humans and animals is one of the key factors leading to this problem. Therefore, special antibi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/04
Inventor 吴范宏赵敏王飞杨兵俞晓东
Owner SHANGHAI ECUST BIOMEDICINE CO LTD
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