反应详情

A mixture of 5α-androst-2-ene-11,17-dione (37.2 g), m-chloroperbenzoic acid (30 g) and chloroform (600 ml) was allowed to stand for 0.5 hour at room temperature before partitioning between chloroform and saturated aqueous NaHCO3 solution. The organic phase was isolated and washed with water, dried and evaporated to a low volume. Addition of petroleum ether (b.p. 60°-80° C.) followed by refrigeration overnight afforded crystalline material (27.5 g). Recrystallisation from ethyl acetate-petroleum ether (b.p. 60°-80° C.) afforded the title compound, m.p. 166°-167°, [α]D +126°.

1. custombefore partitioning between chloroform and saturated aqueous NaHCO3 solution
2. customThe organic phase was isolated
3. washwashed with water
4. customdried
5. customevaporated to a low volume
6. additionAddition of petroleum ether (b.p. 60°-80° C.)
7. waitfollowed by refrigeration overnight