HRID621620
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
0.560 g of 1β,7α-dimethyl-16α-fluoro-6-methylenandrost-4-ene-3,17-dione and 0.59 g of dichlorodicyanobenzoquinone is refluxed in 20 ml of anhydrous dioxane for about 15 hrs. The the reaction mixture is filtered, the solvent removed in vacuo, the residue dissolved in ethyl acetate, the organic layer washed with water, dried over sodium sulfate and the solvent evaporated under vacuum. The crude product is chromatographed on silica gel using hexane/ethyl acetate 40% as eluant to yield 0.42 g of pure 1,7α-dimethyl-16α-fluoro-6-methylenandrosta-1,4-diene-3,17-dione.
WORKUP
后处理
- filtrationThe the reaction mixture is filtered
- customthe solvent removed in vacuo
- dissolutionthe residue dissolved in ethyl acetate
- washthe organic layer washed with water
- dry with materialdried over sodium sulfate
- customthe solvent evaporated under vacuum
- customThe crude product is chromatographed on silica gel