反应详情

The product from Example 36b (1.46 g, 7.6 mmol) was dissolved in methanol (20 mL) to which was added at room temperature sodium carbonate as a 3N solution (35 mL) followed by hydrogen peroxide as a 15% solution (35 mL). The reaction was allowed to stir for 4.5 hours then partitioned by the addition of ethyl acetate and solid sodium chloride. The aqueous phase was extracted several times with ethyl acetate and the combined organics stirred with solid sodium bisulfite followed by drying over MgSO4, filtered and concentration under vacuum to give the title compound (1.36 g, 85%) sufficiently pure for use as isolated.

1. customthen partitioned by the addition of ethyl acetate and solid sodium chloride
2. extractionThe aqueous phase was extracted several times with ethyl acetate
3. stirringthe combined organics stirred with solid sodium bisulfite
4. dry with materialby drying over MgSO4
5. filtrationfiltered
6. concentrationconcentration under vacuum