反应详情

Hydroxylamine hydrochloride (4 g) was added to a water cooled solution of sodium hydroxide (50%; 16 ml). This mixture was added to a solution of 3α-hydroxy-11-oxo-5α-androstane-17β-carboxylic acid (1.5 g) in ethanol (70 ml). The mixture was heated at reflux for 24 h, cooled and brought to pH 1 with concentrated HCl solution. Water (800 ml) was added and the precipitate (1.42 g) was collected by filtration, washed with water (2×300 ml) and dried. Crystallisation from ethyl acetate gave the title compound (1 g) m.p. 250°-253° C. (dec) [α]D +124° (EtOH C=1%).

1. temperatureThe mixture was heated
2. temperatureat reflux for 24 h
3. temperaturecooled
4. filtrationthe precipitate (1.42 g) was collected by filtration
5. washwashed with water (2×300 ml)
6. customdried
7. customCrystallisation from ethyl acetate