반응 #350148

반응 방정식

3,3-ethylenedioxy-17β-hydroxy-1α-methyl-5α-androstane

aluminium

ether

→

3,3-ethylenedioxy-1α-methyl-5α-androstan-17-one

수율 93.3%

용매

toluene

toluene

cyclohexanone

반응 조건

후처리

1. 1
   온도the mixture was heated for 3 hours with slow distillation
2. 2
   세척washed with ice-cold dilute sulphuric acid and water
3. 3
   기타evaporated
4. 4
   workup.DISTILLATIONthe residue steam-distilled
5. 5
   추출After extraction with methylene chloride
6. 6
   기타the resulting product was recrystallised from diisopropyl ether

실험 절차

55 g of 3,3-ethylenedioxy-17β-hydroxy-1α-methyl-5α-androstane in 550 ml of toluene and 110 ml of cyclohexanone were treated at boiling with a solution of 5.5 g of aluminium isopropylate in 55 ml of toluene and the mixture was heated for 3 hours with slow distillation. The mixture was then treated with ether, washed with ice-cold dilute sulphuric acid and water, evaporated and the residue steam-distilled. After extraction with methylene chloride, the resulting product was recrystallised from diisopropyl ether to give 51 g of 3,3-ethylenedioxy-1α-methyl-5α-androstan-17-one of melting point 155.5°-156.6° C.

출처