反应详情

A mixture of 3-(4-piperidinyl)-6-fluorobenzisoxazole (3.42 g, 15 mmol), N-(2-bromoethoxy)-phthalimide (4.3 g, 16 mmol) and K2CO3 (26 g, 18 mmol) in acetonitrile (150 ml) was heated at reflux for 2 hours. The solids were removed and the solvent was evaporated. The residue was purified over a flash chromatography column (packed with SiO2, 60 g: eluted with dichloromethane (DCM) and 1% CH3OH in DCM. The pure product thus obtained, weighing 6.8 g was crystallized from DCM:ethanol. Recrystallization from ethanol and i-propyl ether yielded white crystals (2.4 g, m.p. 125°-127° C.) as the hemihydrate. ANALYSIS: Calculated for C22H20N3O4.0.5.H2O: 63.15%C 5.05%H 10.04%N 2.15%H2O Found: 63.20%C 5.16%H 9.80%N 2.32%H2O

1. temperaturewas heated
2. temperatureat reflux for 2 hours
3. customThe solids were removed
4. customthe solvent was evaporated
5. customThe residue was purified over a flash chromatography column (
6. washeluted with dichloromethane (DCM) and 1% CH3OH in DCM
7. customThe pure product thus obtained
8. customwas crystallized from DCM
9. customRecrystallization from ethanol and i-propyl ether yielded white crystals (2.4 g, m.p. 125°-127° C.) as the hemihydrate