反应详情

Compound 6 (17.8 mmol), sodium tungstate (587 mg, 1.78 mmol), 30% hydrogen peroxide (8.07 mL, 71.2 mmol), methanol (20 mL), and ethyl acetate (200 mL) were combined under argon, then heated to reflux for 4 h. The solution was cooled and aqueous sodium hydrosulfite was added. The methanol was removed in vacuo and saturated sodium bicarbonate was added. The resulting suspension was extracted several times with methylene chloride. The combined organic extracts were washed successively with water and brine. The organic layer was dried with anhydrous sodium sulfate then concentrated in vacuo to give Compound 7 as a foam: 5.0 g (13 mmol, 73% (two steps))

1. temperatureheated
2. temperatureto reflux for 4 h
3. temperatureThe solution was cooled
4. customThe methanol was removed in vacuo and saturated sodium bicarbonate
5. additionwas added
6. extractionThe resulting suspension was extracted several times with methylene chloride
7. washThe combined organic extracts were washed successively with water and brine
8. dry with materialThe organic layer was dried with anhydrous sodium sulfate
9. concentrationthen concentrated in vacuo