HRID14472

反应详情

EQUATION

反应方程式

HRID 14472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A stirred mixture of N-[3-(4-chlorophenyl)-8-hydroxy-2-isopropyl-4-oxo-4H-chromen-7-yl]formamide (0.122 g, 0.34 mmol), cesium carbonate (0.444 g, 1.36 mmol, 4 eq.) and 1,3-dibromopropane (0.069 g, 0.34 mmol) in anhydrous N,N-dimethylformamide (3 ml) is heated at 60° C. under a nitrogen atmosphere for 2 h. The mixture is cooled to room temperature and filtered through Celite filter aid. The pad of Celite is washed with ethyl acetate and methylene chloride, and the combined filtrates are evaporated in vacuo to afford a brown solid. This is purified by flash chromatography (cyclohexane/ethyl acetate=9:1 to 4:1) to furnish the title compound as a yellow solid.

WORKUP

后处理

  1. temperatureThe mixture is cooled to room temperature
  2. filtrationfiltered through Celite
  3. filtrationfilter aid
  4. washThe pad of Celite is washed with ethyl acetate and methylene chloride
  5. customthe combined filtrates are evaporated in vacuo
  6. customto afford a brown solid
  7. customThis is purified by flash chromatography (cyclohexane/ethyl acetate=9:1 to 4:1)