HRID277094

反应详情

EQUATION

反应方程式

HRID 277094 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 2.80 g (0.038 mol) sodiumhydride (60% in oil) in 120 ml tetrahydrofurane and 120 ml dimethylformamide were added 21.6 g (0.064 mol) (cyanomethyl)triphenyl-phosphonium chloride. After stirring for 1 hour at room temperature a solution of 4.00 g (0.032 mol) 2-fluoro-4-pyridinecarboxaldehyde in 35 ml tetrahydrofurane were added and stirring was continued for 2 days. Then 30 ml methanol were added, the solvents were evaporated and the residue chromatographed on silicagel with ethylacetate/hexane 1/2 to yield 0.45 g (10%) (E)-and (Z)-3-(2-fluoro-pyridin-4-yl)-acrylonitrile as light yellow solid. MS m/e (%): 148 (M+, 100), 128 (43).

WORKUP

后处理

  1. additionwere added
  2. customthe solvents were evaporated
  3. customthe residue chromatographed on silicagel with ethylacetate/hexane 1/2