反应详情

A mixture of 4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine (11 g, 50 mmol), K2CO3 (8.5 g, 74 mmol) and 3-bromopropionitrile (8.2 g, 1.2 eq) in acetonitrile (300 ml) was heated at reflux for 24 hours. The mixture was cooled and the insolubles were filtered. The solvent was removed on a rotary evaporator and the crude product was purified by flash chromatography over a silica gel column (SiO2, 120 g). The product thus purified weighed 8.94 g. Recrystallization from ethanol yielded the nitrile as white crystals 4.3 g, m.p. 100°-101° C.

1. temperaturewas heated
2. temperatureat reflux for 24 hours
3. temperatureThe mixture was cooled
4. filtrationthe insolubles were filtered
5. customThe solvent was removed on a rotary evaporator
6. customthe crude product was purified by flash chromatography over a silica gel column (SiO2, 120 g)
7. customThe product thus purified
8. customRecrystallization from ethanol