反应 #93683

反应方程式

17α-Ethynyl-17β-hydroxy-6-β-(N-phenyl-N-ethylaminomethyl)-16-methyleneandrosta-4-en-3-one

17α-Ethynyl-17β-hydroxy-6β-(N-phenyl-N-ethylaminomethyl)-16-methyleneandrosta-4-en-3-one

hydrochloric acid

Water

→

title compound

17α-Ethynyl-17β-hydroxy-6,16-dimethyleneandrosta-4-en-3-one

溶剂

THF

反应条件

后处理

1. 1
   其他the reaction
2. 2
   过滤the mixture filtered
3. 3
   洗涤the solids washed with 10% hydrochloric acid, twice with water, once with 5% sodium bicarbonate, and three times with water to neutrality
4. 4
   其他Solids were then dried under nitrogen overnight

实验过程

17α-Ethynyl-17β-hydroxy-6-β-(N-phenyl-N-ethylaminomethyl)-16-methyleneandrosta-4-en-3-one (Example 3) in THF (20 ml) are mixed. Degassed hydrochloric acid (6N, 55 ml plus 20 ml THF) are added. The mixture is stirred overnight at 20°-25° under nitrogen, at which time TLC shows the reaction to be complete. Water (110 ml) is added, the mixture filtered, the solids washed with 10% hydrochloric acid, twice with water, once with 5% sodium bicarbonate, and three times with water to neutrality. Solids were then dried under nitrogen overnight to give the title compound.

来源