反应详情

A stirred mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.9 g, 17.7 mmol), N,N-dimethyl-4-bromopropoxy-3-methoxybenzamide (5.54 g, 17.5 mmol) and K2CO3 (3 g) in acetonitrile (250 ml) was heated at reflux for one hour. At the end of the reaction, the insolubles were filtered and washed with dichloromethane. The solvent was removed on a rotary evaporator. The residue was purified by flash chromatography over a silica gel column. The product thus obtained as an oil weighed 7 g. Crystallization from hot ethanol (45 ml) afforded analytically pure N,N-dimethyl-4-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propoxy]-3methoxybenzamide, 3.95 g, 50%, as light yellow crystals, m.p.=126°-127° C.

1. temperaturewas heated
2. temperatureat reflux for one hour
3. customAt the end of the reaction
4. filtrationthe insolubles were filtered
5. washwashed with dichloromethane
6. customThe solvent was removed on a rotary evaporator
7. customThe residue was purified by flash chromatography over a silica gel column
8. customThe product thus obtained as an oil
9. customCrystallization from hot ethanol (45 ml)