HRID1953293

反应详情

EQUATION

反应方程式

HRID 1953293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.4 g (77.3 mmol) of 2-coumaranone are dissolved in 200 ml xylene and after the addition of 32 g (77.3 mmol) of 4-cyanobenzyl-triphenylphosphonium chloride and 8.7 g (77.3 mmol) of potassium-tert.butoxide the mixture is refluxed for 3 hours under a nitrogen atmosphere. The solvent is distilled off, the residue is taken up in ethyl acetate, combined with silica gel and concentrated by evaporation. Then it is chromatographed on silica gel and eluted with petroleum ether/ethyl acetate (8:2). The desired fractions are combined and concentrated by evaporation.

WORKUP

后处理

  1. temperatureis refluxed for 3 hours under a nitrogen atmosphere
  2. distillationThe solvent is distilled off
  3. concentrationconcentrated by evaporation
  4. customThen it is chromatographed on silica gel
  5. washeluted with petroleum ether/ethyl acetate (8:2)
  6. concentrationconcentrated by evaporation