HRID1753704

反应详情

EQUATION

反应方程式

HRID 1753704 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 32.5 g (100 mmole) 2,7-dibromo-9H-carbazole, 20.4 g (100 mmole) iodobenzene, 9.5 g (150 mmole) of copper powder, 27.6 g (200 mmole) of potassium carbonate, and 600 ml dimethylformamide were heated at 130° C. under nitrogen overnight, then cooled to room temperature, the solution was filtered. The filtrate was extracted three times with dichloromethane and water, dried with anhydrous magnesium sulfate, the solvent was evaporated in vacuum. The residue was purified by column chromatography on silica(hexane-dichloromethane) afforded a white solid (31.3 g, 78 mmol, 78%).

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. filtrationthe solution was filtered
  3. extractionThe filtrate was extracted three times with dichloromethane and water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customthe solvent was evaporated in vacuum
  6. customThe residue was purified by column chromatography on silica(hexane-dichloromethane)