HRID37199
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed for 48 hours
- customAfter removing the solvent
- extractionthe solid residue was extracted with chloroform
- customThe chloroform solution was evaporated to dryness
- additioneluated with a mixture of diethylether/ethyl acetate(5:1)
- customRemoving the solvents of the collected fractions (Rf=0.39)