反应详情

To a stirred solution of 1,5-androstadiene-3β,17β-diol in a mixture of dry ether and glyme is added zinc-copper couple and methylene iodide. This reaction mixture is refluxed for 4 hours, cooled to room temperature, diluted with ether and filtered. The filtrate is washed with aqueous sodium chloride, water and dried over anhydrous magnesium sulfate. The ether is removed under reduced pressure and the residue crystallized from acetone-hexane to yield 1β,2β-methylene-5-androstene-3β,17β-diol.

1. temperatureThis reaction mixture is refluxed for 4 hours
2. filtrationfiltered
3. washThe filtrate is washed with aqueous sodium chloride, water
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe ether is removed under reduced pressure
6. customthe residue crystallized from acetone-hexane