反应详情

A solution of crude 10 (6.1 mmol) in dichloromethane (80 mL) was treated with manganese dioxide (85%, 8 g, 15 equiv.) and this suspension was stirred at reflux for 3 hr. The solids were filtered out and washed with ethyl acetate. The solvent was removed in a rotary evaporator and the residue was purified by chromatography on silica (80 g) with 5% ethyl acetate in heptane (1 L) and 7.5% ethyl acetate in heptane (3 L) to afford pure 11 (1.64 g, 60% over 2 steps).

1. temperatureat reflux for 3 hr
2. filtrationThe solids were filtered out
3. washwashed with ethyl acetate
4. customThe solvent was removed in a rotary evaporator
5. customthe residue was purified by chromatography on silica (80 g) with 5% ethyl acetate in heptane (1 L) and 7.5% ethyl acetate in heptane (3 L)
6. customto afford pure 11 (1.64 g, 60% over 2 steps)