反应 #94829

反应方程式

hydrochloric acid

21-Chloro-17α-hydroxy-20-methoxypregna-4,9(11),20-trien-3-one

THF

acetone

→

title compound

21-Chloro-17α-hydroxypregna-4,9(11)-diene-3,20-dione

溶剂

methanol

hexane

反应条件

后处理

1. 1
   温度the resulting slurry heated at 40° for 1.5 hours
2. 2
   温度The mixture is cooled to 20°-25°
3. 3
   其他The solids are isolated by filtration
4. 4
   洗涤washed with hexane/ethyl acetate (85/15, 13 ml)

实验过程

21-Chloro-17α-hydroxy-20-methoxypregna-4,9(11),20-trien-3-one (VII, Example 4, 1.0 g), THF (4 ml), acetone (4.9 ml), and methanol (1.4 ml) are mixed. Aqueous hydrochloric acid (6 N, 0.44 ml) is added and the resulting slurry heated at 40° for 1.5 hours. The mixture is cooled to 20°-25° and diluted with hexane (3 ml). The solids are isolated by filtration and washed with hexane/ethyl acetate (85/15, 13 ml) to give the title compound.

来源