반응 #320824

반응 방정식

water

3β-(2-tosyloxyethoxy)-17β-(3-furyl)-5β-androstan-14β-ol

1-(2-aminoethyl)pyrrolidine

→

title compound

3β-(2-(2-(1-Pyrrolidinyl)ethylamino)ethoxy)-17β-(3-furyl)-5β-androstan-14β-ol

용매

ethanol

반응 조건

후처리

1. 1
   온도at reflux under nitrogen for 3 hrs
2. 2
   추출The residue was extracted with methylene chloride
3. 3
   세척the organic layer was washed with water to neutral pH
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   기타evaporated to dryness under reduced pressure
6. 6
   기타The crude residue was purified by flash-chromatography (SiO2)

실험 절차

To a solution of 0.20 g of 3β-(2-tosyloxyethoxy)-17β-(3-furyl)-5β-androstan-14β-ol in 2 ml of absolute ethanol 0.15 g of 1-(2-aminoethyl)pyrrolidine were added. The solution was kept at reflux under nitrogen for 3 hrs, then 10 ml of water were added. The residue was extracted with methylene chloride, the organic layer was washed with water to neutral pH, dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure. The crude residue was purified by flash-chromatography (SiO2) using methylene chloride/methanol 95/5 as eluant to give 0.15 g of the title compound (I-ag).

출처