HRID621620

反应详情

EQUATION

反应方程式

HRID 621620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationThe the reaction mixture is filtered
  2. customthe solvent removed in vacuo
  3. dissolutionthe residue dissolved in ethyl acetate
  4. washthe organic layer washed with water
  5. dry with materialdried over sodium sulfate
  6. customthe solvent evaporated under vacuum
  7. customThe crude product is chromatographed on silica gel