反応 #94829

反応方程式

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

溶媒

methanol

hexane

反応条件

後処理

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
   その他The solids are isolated by filtration
4. 4
   洗浄washed with hexane/ethyl acetate (85/15, 13 ml)

実験手順

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.

出典