反应详情

To a stirred solution of LiAlH4 (1.0 M in THF, 35 mL, 35 mmol), was added a solution of 1a. (2.17 g, 12.4 mmol) in THF (10 mL) for 5 min at 0° C. under nitrogen. The resulting mixture was warmed gradually to reflux, and heated at reflux for 5.5 h. To the cooled mixture with stirring, was added sat'd Na2SO4 dropwise till the complete decomposition of LiAlH4. The mixture was filtered, and rinsed with EtOAc. The organic was washed with H2O, brine, dried (MgSO4), and concentrated to dryness. It was purified by flash chromatography (silica gel, 0-20% EtOAc in hexanes) to give pure 1b (1.86 g, yield: 93%). LC-MS ESI 162 (M+H).

1. temperatureThe resulting mixture was warmed gradually
2. temperatureto reflux
3. temperatureheated
4. temperatureat reflux for 5.5 h
5. filtrationThe mixture was filtered
6. washrinsed with EtOAc
7. washThe organic was washed with H2O, brine
8. dry with materialdried (MgSO4)
9. concentrationconcentrated to dryness
10. customIt was purified by flash chromatography (silica gel, 0-20% EtOAc in hexanes)