反应详情

温度

25 °C

A 3.5 ml portion of acetonitrile was added to 0.570 g of dihydrate of 5-mercapto-1-methyl-1H-tetrazole sodium salt and 0.680 g of 7-ACA, and 1.64 g of diphosphoryl tetrachloride was added dropwise to the mixture under cooling over an external bath at -30° to -20° C., followed by adding 2.29 g of DCPA and rinsing with 0.5 ml of acetonitrile. The reaction solution was stirred at -5° to 0° C. for 5 minutes, warmed at 25° C., and stirred for 40 minutes to allow the reaction to proceed. The reaction solution was cooled and poured into ice-water, which was placed in a refrigerator overnight. The mixture was adjusted to pH 4.0 with 25% aqueous ammonia, and the resultant precipitate was recovered by filtration, washed with cold water and acetone successively and dried, thereby affording 0.732 g (89.3% of yield) of 7-amino-3-(1-methyl-1H-tetrazol-5 -yl)thiomethyl-3-cephem-4-carboxylic acid. The NMR values of the product were in accordance with those of the authentic sample.

1. additionwas added dropwise to the mixture
2. temperatureunder cooling over an external bath at -30° to -20° C.
3. washrinsing with 0.5 ml of acetonitrile
4. stirringstirred for 40 minutes
5. customthe reaction
6. temperatureThe reaction solution was cooled
7. customwas placed in a refrigerator overnight
8. filtrationthe resultant precipitate was recovered by filtration
9. washwashed with cold water and acetone successively
10. customdried