反应详情

To a solution of alcohol compound from Step 2 (400 mg) was added Dess-Martin reagent (500 mg) and the mixture was stirred at rt for 3 h. After the reaction was complete the mixture was diluted with methylene chloride followed by the addition of 0.1 N NaOH aqueous solution (12 mL) and the stirring was continued for about 20 min. The organic phases were washed with 0.1 N NaOH solution, brine, dried over MgSO4, and concentrated under reduced pressure. The residue was purified by flash chromatographed (eluting with 5% methanol in methylene chloride). MS (ESI): 406.1 (M+H+)

1. waitthe stirring was continued for about 20 min
2. washThe organic phases were washed with 0.1 N NaOH solution, brine
3. dry with materialdried over MgSO4
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by flash
6. customchromatographed
7. wash(eluting with 5% methanol in methylene chloride)