反应详情

Under argon atmosphere, (R)-3-(t-butyldiphenylsilyloxy)-2-methylpropanol (48) (725 mg, 2.2 mmol) was dissolved in 40 ml of dry dichloromethane. MS-4A (30 mg), NMO (862 mg, 11.1 mmol) and TPAP (catalytic amount) were added to the resultant solution at 0° C., and the mixture was stirred for 15 min. The reaction mixture was further stirred overnight after the temperature was returned to room temperature. Subsequently, H2O was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with brine, dried over magnesium sulfate and evaporated. The obtained crude product was purified by column chromatography (21 g, 4% AcOEt-hexane) to obtain a colorless oily product (49) (700 mg, 97%).

1. waitThe reaction mixture was further stirred overnight
2. customwas returned to room temperature
3. extractionthe mixture was extracted with ethyl acetate
4. washThe ethyl acetate layer was washed with brine
5. dry with materialdried over magnesium sulfate
6. customevaporated
7. customThe obtained crude product
8. customwas purified by column chromatography (21 g, 4% AcOEt-hexane)