A kind of preparation method of cefmetazole sodium
A technology of cefmetazole sodium and mercaptotetrazolium, which is applied in the direction of organic chemistry and can solve the problems of high cost, numerous process steps, and low yield
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[0024] Add 132ml (141.1g, 1.57mol) dimethyl carbonate and 162g boron trifluoride dimethyl carbonate complex into a 1000ml four-necked flask, add 21.5g (0.185mol) 1-methyl-carbonate complex at 10-12°C 5-Mercaptotetrazolium, add 50g (0.184mol) 7-aminocephalosporanic acid (7-ACA) after stirring for 10min, react at 25°C for 45min, cool to 0°C, add dropwise 32g (0.283mol) ethyl chloride Acyl chloride, then add 37ml N'N-dimethylformamide dropwise, keep the temperature for 45 minutes, add 300ml water and 300ml dimethyl carbonate to the reaction solution, stir evenly, let stand to separate layers, and extract the water layer with 400ml dimethyl carbonate , Combine the dimethyl carbonate layer, add 5g of activated carbon to decolorize for 30min, add triethylamine dropwise to the dimethyl carbonate solution, adjust the pH to 6.8, crystallize at 0-5°C for 2h, filter with suction, and dry the filter cake in vacuum at 45°C , to obtain 67g (0.180mol) of 7-aminoceftrizime (7-ACT), yield 98%....
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