HCID 86733148, compound → HCID 86733140, compound

Participants

Reaction Steps

A solution of 17β-carbamoyl-5α-androstan-3-one (2.4 g.) and polyphosphate ester (12 g.) in chloroform (125 ml.) was refluxed for 24 hours. After removing the chloroform by evaporation aqueous 10% sodium carbonate (100 ml.) was added, the mixture cooled, and extracted with ether. The ethereal extracts were washed with water, dried (MgSO4), filtered and evaporated to afford a buff solid (2.45 g.). Purification by preparative t.l.c. (ethanol/chloroform 1:19) afforded a solid (1.48 g.) which was further purified by passing through a florisil column and crystallisation from dichloromethane/petrol to give title compound (915 mg.) m.p. 150°-152°; [α]D + 89° (c 1.12%).

Provenance & Evidence