反应详情

Acetone cyanohydrin (1.37 ml) is added to a mixture of 9α-hydroxyandrost-4-ene-3,17-dione (0, U.S. Pat. No. 3,065,146, 3.024 g) in methanol (10 ml). The mixture is stirred at about 35°-39° for about 2 hr, then at about 4°-54° for 1.25 hr. 0.1 ml of a potassium cyanide solution (1 g in 2.0 ml of water) is added and the mixture stirred at about 50°-55° for 30 min and then allowed to stand at 20°-25° overnight. The solids are collected, washed well with methanol and dried under reduced pressure at about 55° for 3 hr to give the title compound, NMR (CDCl3 /DMSO-d6 ; 10/1) 5.8, 2.4, 1.3 and 1.0 δ.

1. waitat about 4°-54° for 1.25 hr
2. stirringthe mixture stirred at about 50°-55° for 30 min
3. waitto stand at 20°-25° overnight
4. customThe solids are collected
5. washwashed well with methanol
6. customdried under reduced pressure at about 55° for 3 hr