反应详情

温度

10 °C

Mixed were 1.36 g of 7-ACA, 0.36 g of water and 1.32 g of 2-dimethylaminocarbonylmethyl-5-mercapto-1,3,4-thiadiazole, and 6.5 ml of acetonitrile was added. 5.04 g of diphosphoryl tetrachloride was added through a dropping funnel to the mixture at -20° to -30° C., followed by rinsing the funnel with 1.5 ml of acetonitrile. The reaction mixture was warmed at 10° C. over a period of 5 minutes with stirring, placed in a warm water bath of 40° C. and stirred at the same temperature for 20 minutes. The reaction solution was cooled with ice and adjusted to pH 4.1 with aqueous concentrated ammonia after the addition of 10 ml of cold water. The precipitate was recovered by filtration, washed with water and dried, thereby affording 1.82 g (87.6%) of 7-amino-3-(2-dimethylaminocarbonylmethyl-1,3,4-thiadiazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid.

1. additionMixed
2. additionwas added
3. washby rinsing the funnel with 1.5 ml of acetonitrile
4. customplaced in a warm water bath of 40° C.
5. stirringstirred at the same temperature for 20 minutes
6. temperatureThe reaction solution was cooled with ice
7. additionafter the addition of 10 ml of cold water
8. filtrationThe precipitate was recovered by filtration
9. washwashed with water
10. customdried