反应详情

A 320 ml portion of acetonitrile was added to 54.5 g of 7-ACA and 25,6 g of 5-mercapto-1-methyl-1H-tetrazole, and 296.7 g of DCPA was added to the mixture with stirring and under cooling at -20° to -10° C. After the dissolution, the reaction mixture was stirred at 15° to 17° C. for 40 minutes to allow the reaction to proceed, cooled and poured into 1.8 kg of ice-water. The mixture was allowed to stand at 5° C. overnight, cooled by adding ice under stirring and adjusted to pH 4.0 with 25% aqueous ammonia. The resulting precipitate was recovered by filtration, washed with 480 ml of cold water and 500 ml of acetone successively, and dried, thereby affording 62.2 g (94.7% of yield) of 7-amino-3-(1-methyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid.

1. additionwas added to the mixture
2. temperatureunder cooling at -20° to -10° C
3. dissolutionAfter the dissolution
4. stirringthe reaction mixture was stirred at 15° to 17° C. for 40 minutes
5. customthe reaction
6. temperaturecooled
7. temperaturecooled
8. additionby adding ice
9. stirringunder stirring
10. filtrationThe resulting precipitate was recovered by filtration
11. washwashed with 480 ml of cold water and 500 ml of acetone successively
12. customdried