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.

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 (packed with SiO2, 60 g; eluted with dichloromethane (DCM) and 1% CH3OH in DCM)
6. customThe pure product thus obtained
7. customwas crystallized from DCM
8. customRecrystallization from ethanol and i-propyl ether yielded white crystals (2.4 g, m.p. 125°-127° C.) as the hemihydrate