反应详情

A mixture of 4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine (11 g, 50 mmol), K2CO3 (8.5 g, 61.6 mmol) and 2-chloroacetonitrile (5.5 g, 73 mmol) in acetonitrile (250 ml) was heated at reflux for 24 hours. The insolubles were filtered off and rinsed with methylene chloride (DCM). During concentration of the solvents on the rotary evaporator, crystals appeared. The crystals were collected and weighed 5.79 g. The product in the mother liquor was further purified by flash chromatography over a silica gel column (SiO2, 70 g; eluted with DCM, and 1%CH3OH in DCM). The second crop of product thus obtained weighed 5.2 g. The total yield was 10.9 g. The sample was recrystallized once more form ethanol, m.p. 130°-132° C.

1. temperaturewas heated
2. temperatureat reflux for 24 hours
3. filtrationThe insolubles were filtered off
4. washrinsed with methylene chloride (DCM)
5. customDuring concentration of the solvents on the rotary evaporator, crystals
6. customThe crystals were collected
7. customThe product in the mother liquor was further purified by flash chromatography over a silica gel column (SiO2, 70 g; eluted with DCM, and 1%CH3OH in DCM)
8. customThe second crop of product thus obtained
9. customThe sample was recrystallized once more
10. customform ethanol, m.p. 130°-132° C.