反応 #52574

反応方程式

E-17-chloromethylen-estr-4-en-3-one

hydrogen peroxide

sodium hydroxide

→

E-17-Chloromethylene-4ξ,5ξ-epoxy-estran-3-one

溶媒

methanol

methylene chloride

反応条件

後処理

1. 1
   workup.ADDITIONAfter dropwise addition
2. 2
   温度the temperature is slowly increased to room temperature
3. 3
   その他After about 1.5 hours of reaction time
4. 4
   抽出extracted with methylene chloride
5. 5
   その他The combined extracts are dried on sodium sulfate
6. 6
   濃縮concentrated by evaporation
7. 7
   その他1.1 g of a white, sticky foam is obtained

実験手順

3.93 mmol (1.2 9) of E-17-chloromethylen-estr-4-en-3-one is dissolved in a mixture of 12 ml of methanol and 10 ml of methylene chloride under a cover gas (argon) and cooled to 0° C. 9.2 mmol (0.94 ml) of hydrogen peroxide (30%) and 1.65 mmol (0.4 ml) of sodium hydroxide solution (c=4 mol/l) are added in drops in succession to the cooled solution while being stirred. After dropwise addition is completed, the temperature is slowly increased to room temperature. After about 1.5 hours of reaction time, the mixture is added to ice water and extracted with methylene chloride. The combined extracts are dried on sodium sulfate and concentrated by evaporation. 1.1 g of a white, sticky foam is obtained.

出典