反应详情

Bromine (1.2 ml) was added to a mixture of 9a-acetyl-1,2,3,4,4a,9a-hexahydrofluoren-9-one (5 g) in methanol (20 ml) at 20-30° C. The reaction mixture was stirred for 2 hours and quenched with NaHCO3 solution (0.8 g NaHCO3 and 24 ml water). The mixture was extracted with CH2Cl2 (3×30 ml) and the organic phase was washed with water (30 ml) and dried over Na2SO4. Evaporation gave 6.6 g of the crude product which was used without further purification for the next step.

1. customquenched with NaHCO3 solution (0.8 g NaHCO3 and 24 ml water)
2. extractionThe mixture was extracted with CH2Cl2 (3×30 ml)
3. washthe organic phase was washed with water (30 ml)
4. dry with materialdried over Na2SO4
5. customEvaporation