Preparation method of cefazolin sodium with previous research quality and medicine preparation of cefazolin sodium
A technology for cefazolin sodium and preparation, which is applied in the field of preparation of the original development quality cefazolin sodium, can solve the problems of cefazolin sodium solvent residue and high water content, high production cost, reduced production efficiency, etc. The effect of using freeze-drying technology to control solvent residues and improve production efficiency
Active Publication Date: 2016-05-04
广东金城金素制药有限公司 +1
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Abstract
The invention discloses a preparation method of cefazolin sodium with previous research quality. The preparation method is characterized by comprising the following steps: (1) adding a boron trifluoride-dimethyl carbonate solution into dimethyl carbonate; stirring and adding 2-sulfydryl-5-methyl-1,3,4-thiadiazole and 7-ACA (Acetic Acid) to react; after the reaction is finished, adding dimethyl formamide and dropwise adding hydrochloric acid; adjusting the temperature to 25 to 35 DEG C and reacting for 60 minutes; filtering and washing with acetone; drying in vacuum to obtain a TDA (Toluene Diamine) crude product; (2) preparing mixed anhydride from dichloromethane, tetrazolyl acetic acid, triethylamine and pivaloyl chloride; (3) adding the TDA crude product into a dichloromethane solvent; cooling and dropwise adding tetramethyl guanidine; dropwise adding the mixed anhydride to react, and purifying and refining a crystal through a low-temperature acetonitrile-water extraction process after extraction and crystallization. With the adoption of the preparation method provided by the invention, the moisture content of the product can be reduced and residues of the solvent can be reduced; the increasing of related substances can be effectively reduced, a freeze-drying technology is not used and the production efficiency is improved.
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Powder deliveryOrganic chemistry
Technology Topic
DiamineDimethyl formamide +22
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