反应详情

温度

20 °C

Phenyl chloroformate (16.4 g.) is run, over the course of 10 minutes, at a temperature of about 20° C., into a suspension of 5-hydroxy-6-(5-methylpyrid-2-yl)-7-oxo-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazine (8.47 g.) in anhydrous pyridine (110 cc.). The reaction mixture is stirred for 3 hours at a temperature of about 20° C. and is then cooled to a temperature of about 5° C. Water (350 cc.) is then added over the course of 15 minutes. The insoluble product is filtered off, washed with water (4×50 cc.), acetonitrile (2×25 cc.) and diisopropyl ether (2×30 cc.). After drying, 6-(5-methylpyrid-2-yl)-7-oxo-5-phenoxycarbonyloxy-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazine (11.8 g.), which melts at 176° C., is obtained.

1. temperatureis then cooled to a temperature of about 5° C
2. filtrationThe insoluble product is filtered off
3. washwashed with water (4×50 cc.), acetonitrile (2×25 cc.) and diisopropyl ether (2×30 cc.)
4. customAfter drying