反应详情

温度

20 °C

Anhydrous piperazine (86 g.) is added to a suspension of 6-(5-chloropyrid-2-yl)-7-oxo-5-phenoxycarbonyloxy-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazine (76.4 g.) in acetonitrile (760 cc.). The reaction mixture is stirred for 5 hours at a temperature of about 20° C. and then the insoluble product is filtered off, washed with acetonitrile (3×25 cc.) and with diisopropyl ether (50 cc.). After drying, a product (30.8 g.) is obtained and is dissolved in methylene chloride (750 cc.). A small amount of insoluble matter is removed by treating the solution with decolourising charcoal (2 g.). After filtration, the solution is concentrated to dryness under reduced pressure. 6-(5-Chloropyrid-2-yl)-7-oxo-5-(piperazin-1-yl)carbonyloxy-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazine (28.3 g.), which melts at 205° C., is thus obtained.

1. filtrationthe insoluble product is filtered off
2. washwashed with acetonitrile (3×25 cc.) and with diisopropyl ether (50 cc.)
3. customAfter drying
4. customa product (30.8 g.) is obtained
5. customA small amount of insoluble matter is removed
6. additionby treating the solution with decolourising charcoal (2 g.)
7. filtrationAfter filtration
8. concentrationthe solution is concentrated to dryness under reduced pressure