HRID1953293
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureis refluxed for 3 hours under a nitrogen atmosphere
- distillationThe solvent is distilled off
- concentrationconcentrated by evaporation
- customThen it is chromatographed on silica gel
- washeluted with petroleum ether/ethyl acetate (8:2)
- concentrationconcentrated by evaporation