Sodium Hydroxide → HCID 86736928, compound

Participants

Reaction Steps

A solution of (Z)-3α-hydroxy-5α-pregn-17(20)-en-11-one (10.264 g) in warm industrial methylated spirits (320 ml) was heated with hydroxylamine hydrochloride (3.25 g) and sodium hydroxide (5.123 g) in water (10 ml). The mixture was refluxed for 41 hours and, after addition of more hydroxylamine hydrochloride (15.35 g) in water (20 ml) and sodium hydroxide (25.04 g) in water (50 ml) refluxing was continued for a further 6 hours. The mixture was then poured into water and the crystalline material (10.419 g) collected by filtration. Crystallisation of a portion from aqueous ethanol afforded an analytical sample of title compound m.p. 233°-235°.

Provenance & Evidence