반응 #52574

반응 방정식

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

hydrogen peroxide

sodium hydroxide

→

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

용매

methanol

methylene chloride

반응 조건

후처리

1. 1
   workup.ADDITIONAfter dropwise addition
2. 2
   온도the temperature is slowly increased to room temperature
3. 3
   기타After about 1.5 hours of reaction time
4. 4
   추출extracted with methylene chloride
5. 5
   기타The combined extracts are dried on sodium sulfate
6. 6
   농축concentrated by evaporation
7. 7
   기타1.1 g of a white, sticky foam is obtained

실험 절차

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.

출처