반응 #459001

반응 방정식

lithium tri-t-butoxy-aluminum hydride

17β,19-dihydroxyandrost-4-en-3-one diacetate

sodium potassium tartrate

→

androst-4-ene-3β,17β,19-triol 17,19-diacetate

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   여과The mixture is filtered
2. 2
   농축concentrated to a small volume under reduced pressure
3. 3
   세척washed well with water
4. 4
   건조The combined ether extracts are dried over magnesium sulfate
5. 5
   여과filtered
6. 6
   기타the ether removed under vacuum
7. 7
   기타to yield a residue which when
8. 8
   기타recrystallized from a mixture of acetone-hexane

실험 절차

To a solution of lithium tri-t-butoxy-aluminum hydride in tetrahydrofuran is added a tetrahydrofuran solution of 17β,19-dihydroxyandrost-4-en-3-one diacetate. The resulting mixture is stirred at 20° C. for a period of 18 hours after which is added an aqueous solution of sodium potassium tartrate. The mixture is filtered and concentrated to a small volume under reduced pressure. The concentrate is taken up in ether and washed well with water. The combined ether extracts are dried over magnesium sulfate, filtered and the ether removed under vacuum to yield a residue which when recrystallized from a mixture of acetone-hexane results in the preparation of the desired androst-4-ene-3β,17β,19-triol 17,19-diacetate.

출처