反应详情

A 4.0 ml portion of acetonitrile was added to 0.826 g of 7-amino-3-(3-carboxypropionyloxy)methyl-3-cephem-4-carboxylic acid and 0.32 g of 5-mercapto-1-methyl-1H-tetrazole, and 3.71 g of DCPA was added through a dropping funnel to the mixture under cooling at -5° to 0° C., followed by rinsing the funnel with 0.5 ml of acetonitrile. The mixture was stirred at the same temperature and turned into a solution. Then, the reaction solution was stirred for 45 minutes at 14° to 15° C. to allow the reaction to proceed. The reaction solution was cooled with ice, and poured into ice-water, which was placed in a refrigerator overnight and adjusted to pH 4.0 with 25% aqueous ammonia. The precipitated powder was recovered by filtration, washed with water and acetone successively, and dried, thereby affording 0.722 g (88.0% of yield) of 7-amino-3-(1-methyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid. The IR and NMR values of the product were in accordance with those of the authentic sample.

1. additionwas added through a dropping funnel to the mixture
2. temperatureunder cooling at -5° to 0° C.
3. washby rinsing the funnel with 0.5 ml of acetonitrile
4. stirringThen, the reaction solution was stirred for 45 minutes at 14° to 15° C.
5. customthe reaction
6. temperatureThe reaction solution was cooled with ice
7. customwas placed in a refrigerator overnight
8. filtrationThe precipitated powder was recovered by filtration
9. washwashed with water and acetone successively
10. customdried