반응 #93683

반응 방정식

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

용매

THF

반응 조건

후처리

1. 1
   기타the reaction
2. 2
   여과the mixture filtered
3. 3
   세척the solids washed with 10% hydrochloric acid, twice with water, once with 5% sodium bicarbonate, and three times with water to neutrality
4. 4
   기타Solids were then dried under nitrogen overnight

실험 절차

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.

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