反应详情

DDQ (10 mg, 0.041 mmol) was added to a mixture of 15-5 (11 mg, 0.021 mmol) in dichloromethane (0.5 mL)/water (25 μL). After 1 h, dichloroethane (0.5 mL) was added and the reaction was stirred overnight. Saturated NaHCO3 solution was added and the resulting mixture was extracted with dichloromethane (3×20 mL). The combined dichloromethane solution was washed with brine and then was dried (Na2SO4), filtered and evaporated. Purification of the residue by flash chromatography on silica gel (60% ethyl acetate/hexanes) gave 15-8 (5 mg, 59%).

1. extractionthe resulting mixture was extracted with dichloromethane (3×20 mL)
2. washThe combined dichloromethane solution was washed with brine
3. dry with materialwas dried (Na2SO4)
4. filtrationfiltered
5. customevaporated
6. customPurification of the residue by flash chromatography on silica gel (60% ethyl acetate/hexanes)