反应详情

To a solution of compound 14 (0.375 g, 1.05 mmol) in 30 ml of acetone was added 3 ml of CrO3 in 35% H2SO4 at 0° C. The resulted solution was stirred another 2 h at same temperature. Ice water was added. The solution was extracted with ethyl acetate three times. The combined organic phase was washed with brine, followed by drying over Na2SO4. Removal of the solvent afforded the desired product in the yield of 82%. 1HNMR(CDCl3): 8.5-7.8 (m, 6H), 6.8 (s, 1H), 4.08 (s, 2H), 3.8 (s, 3H), 2.24 (s, 3H), 2.21 (s, 3H).

1. extractionThe solution was extracted with ethyl acetate three times
2. washThe combined organic phase was washed with brine
3. dry with materialby drying over Na2SO4
4. customRemoval of the solvent