反应详情

A stirred mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.0 g, 13.6 mmol), K2CO3 (2.45 g, 17.7 mmol), 2-methanesulfonyloxymethyl-1,4-benzodioxan (3.35 g, 13.7 mmole) in acetonitrile (100 ml) was heated at reflux for 12 hours. At the end of the reaction, the insolubles were filtered and rinsed with dichloromethane. The organic solution was concentrated. The crude oil was purified by flash chromatography on a silica gel column. The fractions containing the pure product were pooled and concentrated to a light yellow oil (3.94 g, 74%). Crystallization from ethanol and petroleum ether gave 2-[4-(6-fluoro-1,2-benzisoxazol3-yl)-1-piperidinyl]methyl-1,4-benzodioxan as off-white crystals, 2.22 g, m.p.=86°-87° C.

1. temperaturewas heated
2. temperatureat reflux for 12 hours
3. customAt the end of the reaction
4. filtrationthe insolubles were filtered
5. washrinsed with dichloromethane
6. concentrationThe organic solution was concentrated
7. customThe crude oil was purified by flash chromatography on a silica gel column
8. additionThe fractions containing the pure product
9. concentrationconcentrated to a light yellow oil (3.94 g, 74%)
10. customCrystallization from ethanol and petroleum ether