反应详情

A solution of sodium borohydride (4.12 g) in water (41 ml) was added to a refluxing solution of 20,20-ethylenedioxy-3α-hydroxy-16α-methyl-5α-pregnan-11-one (7.55 g) in ethanol (375 ml) containing pyridine (7 drops). The mixture was refluxed for 1 hr. then cooled and glacial acetic acid added until no further effervescence occurred. The mixture was partitioned between 3%-aqueous sodium hydrogen carbonate and ethyl acetate. The aqueous portion was extracted with additional ethyl acetate. The combined organic extracts were washed with saturated brine solution, dried and evaporated to a white foam which crystallised from acetone-water to afford the title compound as white prisms (3.29 g),

1. temperatureThe mixture was refluxed for 1 hr
2. temperaturethen cooled
3. customThe mixture was partitioned between 3%-aqueous sodium hydrogen carbonate and ethyl acetate
4. extractionThe aqueous portion was extracted with additional ethyl acetate
5. washThe combined organic extracts were washed with saturated brine solution
6. customdried
7. customevaporated to a white foam which
8. customcrystallised from acetone-water