反应详情

Glacial acetic acid (2.87 ml) is added to 9α-hydroxyandrost-4-ene-3,17-dione (0, 13.49 g) and potassium cyanide (4.98 g) slurried in methanol (45 ml) and stirred at 20°-25°. Glacial acetic acid (0.92 ml) is added followed by water (30 ml) over 13.7 hr via a syringe pump, keeping the mixture at 27°. The mixture is stirred an additional 2 hr at 27°. Additional glacial acetic acid (1.5 ml) is added at 15° followed by water (50 ml) at 10°. The mixture is stirred at 10° for 20 min and the product collected by vacuum filtration and washed with water. The solid is dried in an air stream for 24 hr to give the title compound, mp 229°-230°.

1. customat 27°
2. stirringThe mixture is stirred an additional 2 hr at 27°
3. stirringThe mixture is stirred at 10° for 20 min
4. filtrationthe product collected by vacuum filtration
5. washwashed with water
6. customThe solid is dried in an air stream for 24 hr