HRID1603923

反应详情

EQUATION

反应方程式

HRID 1603923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of potassium carbonate (330 mg, 2.39 mmol) in dry N,N-dimethylformamide (15 ml) was added with ethyl 8-hydroxy-4-oxo-4H-1-benzopyran-2-carboxylate (520 mg, 2.39 mmol) stirring at room temperature for 10 min. After that the reaction mixture was added with 4-(4-phenylbutoxy)benzyl chloride 595 mg, 2.17 mmol) and left under stirring at 60° C. for 18 h, subsequently was added with water (25 ml), extracted with ethyl ether (3×50 ml), dried and the solvent was evaporated off under reduced pressure, to obtain a residue which was purified by chromatography through a silica gel column, eluting with petroleum ether:chloroform, 7:3, recovering 740 mg of the title compound (66% yield).

WORKUP

后处理

  1. waitleft
  2. stirringunder stirring at 60° C. for 18 h
  3. extractionextracted with ethyl ether (3×50 ml)
  4. customdried
  5. customthe solvent was evaporated off under reduced pressure
  6. customto obtain a residue which
  7. customwas purified by chromatography through a silica gel column
  8. washeluting with petroleum ether