2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → HCID 18632036, compound

Participants

Reaction Steps

The organic layer is washed with sodium bicarbonate solution, dried and evaporated in vacuo. The residue is purified by column chromatography on silica gel thus giving pure 16α-fluoro-1β-methyl-7-methylenandrost-4-ene-3,17-dione (198 mg). 16α-fluoro-1β-methyl-7-methylenandrost-4-ene-3,17-dione (331 mg) and dichlorodicyanobenzoquinone (363 mg) are refluxed in dioxane solution (20 ml) for about 15 hrs. Then the precipitate is filtered off and the filtrate evaporated in vacuo. The residue is taken up in ethyl acetate and the organic solution washed, dried and evaporated in vacuo. The residue is chromatographed on silica gel using hexane/ethyl acetate as eluant to give pure 16α-fluoro-1-methyl-7-methylenandrosta-1,4-diene-3,17-dione (230 mg).

Provenance & Evidence