反应详情

To a stirred solution of 66.16D (0.350 g, 0.9 mmol) in THF (9 mL, 0.9 mmol) at 0° C. was added LAH in THF (2 mL, 2 mmol, 1.0M). The reaction was stirred for 1 hour. 1N NaOH(aq) was then added to quench the reaction. The reaction was extracted three times with EtOAc. After drying over anhydrous magnesium sulfate and filtering, the organic solvent was removed under reduced pressure and the product was then purified on silica gel (0-20% EtOAc in hexanes) to yield 66.16E as a colorless oil (0.387 g, 120% yield).

1. customto quench
2. customthe reaction
3. extractionThe reaction was extracted three times with EtOAc
4. dry with materialAfter drying over anhydrous magnesium sulfate
5. filtrationfiltering
6. customthe organic solvent was removed under reduced pressure
7. customthe product was then purified on silica gel (0-20% EtOAc in hexanes)