HRID37199

反应详情

EQUATION

反应方程式

HRID 37199 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.4 g (1.5 mmol) 2-cyano-7-(3-chloropropyloxy)-4-oxo-4H-1-benzopyran, 0.38 g (1.5 mmol) 4-diphenylmethylenepiperidine, 0.225 g (1.5 mmol) sodium iodide and 0.21 g (1.5 mmol) potassium carbonate in 200 ml dry acetone was refluxed for 48 hours. After removing the solvent, the solid residue was extracted with chloroform. The chloroform solution was evaporated to dryness and the residue was put on a silica gel column and eluated with a mixture of diethylether/ethyl acetate(5:1). Removing the solvents of the collected fractions (Rf=0.39) afforded the compound (6), 2-cyano-7-[3-(4-diphenylmethylenepiperidin-1-yl)propyloxy]-4-oxo-4H-benzopyran as a thick colorless oil (yield: 79%).

WORKUP

后处理

  1. temperaturewas refluxed for 48 hours
  2. customAfter removing the solvent
  3. extractionthe solid residue was extracted with chloroform
  4. customThe chloroform solution was evaporated to dryness
  5. additioneluated with a mixture of diethylether/ethyl acetate(5:1)
  6. customRemoving the solvents of the collected fractions (Rf=0.39)