反应详情

温度

65 °C

A stirred mixture of 4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine (5.5 g, 25 mmol) and 1,2-expoxybutane (1.89 g, 26.3 mmol) in isopropyl alcohol (100 ml) was heated at 65° C. for 2 days. This mixture was cooled and the solvent was removed to leave a brown oil which was purified by flash chromatography over a silica gel column (SiO2, 70 g; eluted with DCM, 1 1 and MeOH:DCM 2%: 98%) to give an off-white solid weighing 6.3 g. Recrystallization from hot ethanol yielded 1.96 g of fine crystals, m.p. 87°-88° C.

1. temperatureThis mixture was cooled
2. customthe solvent was removed
3. customto leave a brown oil which
4. customwas purified by flash chromatography over a silica gel column (SiO2, 70 g; eluted with DCM, 1 1 and MeOH:DCM 2%: 98%)
5. customto give an off-white solid
6. customRecrystallization from hot ethanol