反应详情

A solution of 2β-ethoxy-3α-hydroxy-17-methylene-5α-androstan-11-one (1.75 g) in ethanol (50 ml) was added to a mixture of hydroxylamine hydrochloride (3.6 g) in 50% sodium hydroxide solution (14 ml) and the resulting suspension was stirred and refluxed for 35 hours. Most of the solvent was evaporated in vacuo and the residue was partitioned between ethyl acetate and water. Evaporation of the washed organic layer and crystallization of the residue from ethyl acetate afford the title compound (1.4 g), m.p. 97°-99°, [α]D +44.1°.

1. temperaturerefluxed for 35 hours
2. customMost of the solvent was evaporated in vacuo
3. customthe residue was partitioned between ethyl acetate and water
4. customEvaporation of the washed organic layer and crystallization of the residue from ethyl acetate