反应详情

温度

0 °C

To a stirred solution of lithium aluminum hydride (2.28 g) in tetrahydrofuran (120 mL), the compound obtained from step c above (8 g) in tetrahydrofuran (50 mL) was added at 0° C. The reaction mixture was stirred at 0° C. for 3 hours. The reaction mixture was quenched carefully with saturated ammonium chloride solution, filtered through celite, and washed with ethyl acetate. The organic layers were separated, washed with brine, and dried over anhydrous sodium sulfate, and solvents were evaporated under reduced pressure. The crude product was purified by silica gel flash column chromatography using 20% to 30% ethyl acetate in hexane to get the title compound as a white crystalline solid (5.1 g).

1. customThe reaction mixture was quenched carefully with saturated ammonium chloride solution
2. filtrationfiltered through celite
3. washwashed with ethyl acetate
4. customThe organic layers were separated
5. washwashed with brine
6. dry with materialdried over anhydrous sodium sulfate, and solvents
7. customwere evaporated under reduced pressure
8. customThe crude product was purified by silica gel flash column chromatography