反应详情

DDQ (41 mg, 0.18 mmol) was added to a mixture of 15-5 (11 mg, 0.021 mmol) in dichloromethane (3.5 mL)/water (175 μL). After 55 min., saturated NaHCO3 solution was added and the resulting mixture was extracted with dichloromethane (3×50 mL). The combined dichloromethane solution was washed with brine and then was dried (Na2SO4), filtered and evaporated. Purification by flash chromatography on silica gel (50%→60% ethyl acetate/hexanes) gave 15-6 (34 mg, 60%).

1. extractionthe resulting mixture was extracted with dichloromethane (3×50 mL)
2. washThe combined dichloromethane solution was washed with brine
3. dry with materialwas dried (Na2SO4)
4. filtrationfiltered
5. customevaporated
6. customPurification by flash chromatography on silica gel (50%→60% ethyl acetate/hexanes)