反应详情

温度

130 °C

A mixture of the product from step (g) (1.6 g), diethyl carbonate (0.73 ml) and potassium carbonate (0.08 g) was heated at 130° C. for 5 hours. The mixture was cooled, taken up in methanol and the insoluble potassium carbonate filtered off. The filtrate was evaporated in vacuo and the residue eluted through a silica colum using DCM/EtOH/NH4OH (30:8:1) as eluant. The eluate was evaporated in vacuo and the residue recrystallised from isopropanol/ether to give the desired product as a colourless crystalline solid (1.1 g), mp 191°-192° C.

1. temperatureThe mixture was cooled
2. filtrationthe insoluble potassium carbonate filtered off
3. customThe filtrate was evaporated in vacuo
4. washthe residue eluted through a silica colum
5. customThe eluate was evaporated in vacuo
6. customthe residue recrystallised from isopropanol/ether