反应详情

To a stirred solution of the 1,5-androstadiene-3β,17β-diol so prepared in a mixture of dry ether and glyme is added zinc-copper couple and methylene iodide. The mixture is refluxed for a period of about 4 hours, cooled to room temperature, diluted with ether and filtered. The filtrate is washed with an aqueous sodium chloride solution, 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. temperatureThe mixture is refluxed for a period of about 4 hours
2. filtrationfiltered
3. washThe filtrate is washed with an aqueous sodium chloride solution, water
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe ether is removed under reduced pressure
6. customthe residue crystallized from acetone-hexane