反应详情

Dess-Martin periodinane (33.0 mg, 0.077 mmol) was added to a solution of 10b (62.0 mg, 0.077 mmol) and pyridine (31.0 μL, 0.386 mmol) in dichloromethane (1 mL) at room temperature. After 30 min, the reaction mixture was poured into saturated aqueous sodium bicarbonate, and extracted twice with ethyl acetate. The combined organic extracts were washed with water, brine, dried (MgSO4), filtered and concentrated in vacuo. Purification of the crude residue by flash chromatography on silica gel (gradient elution; 20-40% ethyl acetate/hexanes) afforded the title compound 10c.

1. extractionextracted twice with ethyl acetate
2. washThe combined organic extracts were washed with water, brine
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification of the crude residue by flash chromatography on silica gel (gradient elution; 20-40% ethyl acetate/hexanes)