Preparation method of cefazolin sodium intermediate TDA (tolylenediamine)

Abstract

The invention provides a preparation method of a cefazolin sodium intermediate TDA (tolylenediamine), which comprises the following steps: by using acetone, acetonitrile, aether, dimethyl carbonate, dichloromethane or chloroform as a solvent, filling 7-ACA (7-aminocephalosporanic acid) and thia-diazole in a weight ratio of 1:1.2 into a reaction vessel, introducing boron trifluoride gas into the reaction vessel, reacting for 1-8 hours while controlling the temperature in the reaction vessel at 0-50 DEG C until the residual 7-ACA is less than 1%, hydrolyzing and crystallizing the reaction product by using sodium carbonate, sodium bicarbonate or ammonia water, carrying out vacuum filtration, washing, and drying to obtain the finished TDA product. The invention does not use boron trifluoride solid complex in the preparation process, and therefore, does not generate waste liquor containing boron trifluoride, thereby preventing the boron trifluoride solid complex from generating pollution and abundant waste liquor to be recovered in the preparation process. Besides, the invention prevents operating personnel from directly contacting the boron trifluoride solid complex in the whole preparation process, thereby lowering the safety risk in the use process.

Description

technical field [0001] The invention relates to a preparation method of cefazolin sodium intermediate TDA, which belongs to the technical field of TDA preparation. Background technique [0002] 7-amino-3 [2-(5-methyl-1,3,4-thiadiazole)-thiomethyl]-3-cephalosporin-4 hydroxy acid (abbreviated as TDA), is an important compound for the production of cefazolin sodium Intermediates are currently prepared by reacting in solvents with 7-ACA and thiadiazole as raw materials and boron trifluoride solid complexes as catalysts. Due to the large pollution, high energy consumption, and large amount of waste liquid in the preparation process of the boron trifluoride solid complex, and the boron trifluoride solid complex is volatile, corrosive and toxic, during the preparation, transportation and use The safety risk in the process is relatively high. The solvent recovered from the waste liquid in the existing production process cannot be reused in the complexation, resulting in a high cos...

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the problem of large pollution, high energy consumption, and large amount of waste liquid in the preparation process of the boron trifluoride solid complex, and the boron trifluoride solid complex is volatile, corrosive and toxic, In the process of preparation, transportation and use, the problem of greater safety risk, and then provide a preparation method of cefazolin sodium intermediate TDA