反应详情

To a stirred solution of 19-tetrahydropyranyloxy-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 four hours, cooled to room temperature, diluted with ether and filtered. The ether filtrate is washed with an aqueous sodium chloride solution, washed with water, and dried over anhydrous magnesium sulfate. The ether is removed under reduced pressure and the residue which remains is crystallized from an acetone-hexane solution to yield 1β,2β-methylene-19-tetrahydropyranyloxy-5-androstene-3β,17β-diol.

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