反应详情

To a suspension of 2.93 (75 mmol) LiAlH4 in THF (100 ml) is slowly added at 0-10° C. a solution of 13.9 g (50 mmol) of compound 101 in THF (50 ml). After complete addition, the suspension is heated to reflux and kept at this temperature for 5 h. The mixture is cooled in an ice-bath and saturated NH4Cl-solution (25 ml) is added carefully. EtOAc (500 ml) and water (100 ml) is added, the phases separated and the organic layer washed with water (100 ml) and brine (100 ml), dried over Na2SO4, filtered and concentrated under reduced pressure to yield 13.2 g (94%) of the title compound as a white solid.

1. additionAfter complete addition
2. temperaturethe suspension is heated
3. temperatureto reflux
4. temperatureThe mixture is cooled in an ice-bath
5. customthe phases separated
6. washthe organic layer washed with water (100 ml) and brine (100 ml)
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure