反应详情

To a stirred solution of 66.30A (0.500 g, 1.2 mmol) in THF (15.00 mL, 183 mmol) at 0° C. was added LAH in THF (2.3 mL, 2.3 mmol, 1.0M). The reaction was stirred for two hours. 1N NaOH(aq) was added to quench the reaction mixture, and the reaction was then 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 (0-10% EtOAc in hexanes) to yield 66.30B as a colorless oil (0.400 g, 80% yield).

1. customto quench the reaction mixture
2. extractionthe reaction was then extracted three times with EtOAc
3. dry with materialAfter drying over anhydrous magnesium sulfate
4. filtrationfiltering
5. customthe organic solvent was removed under reduced pressure
6. customthe product was then purified on silica gel (0-10% EtOAc in hexanes)