反应详情

To a solution of 14b (24 g) in dry THF (300 ml), LiAlH4 (6.9 g) was added in portions. The mixture was stirred at room temperature for 1.5 hours. Excess LiAlH4 (LAH) was destroyed with saturated Na2SO4 solution. The organic phase was concentrated in vacuo, and the crude product was purified via silica gel column chromatography eluting with methylene chloride. The product was recrystallized from hexane to give 5-fluoro-2-methyl-1H-3-indenyl-(2-hydroxy)ethane (15b) (14.9 g, 63% yield): m.p. 65°-66.5° C.

1. customExcess LiAlH4 (LAH) was destroyed with saturated Na2SO4 solution
2. concentrationThe organic phase was concentrated in vacuo
3. customthe crude product was purified via silica gel column chromatography
4. washeluting with methylene chloride
5. customThe product was recrystallized from hexane