HRID1618829

反应详情

EQUATION

反应方程式

HRID 1618829 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
155 °C

PROCEDURE

实验过程

A mixture of carbazole (300 mg, 1.81 mmol), 4,4′-dibromobiphenyl (846 mg, 2.71 mmol), copper (344 mg, 5.43 mmol), 18-crown-6 (187 mg, 0.71 mmol), potassium carbonate (750 mg, 5.43 mmol), and anhydrous N,N-dimethylformamide (10 mL) was degassed for 30 minutes. The resulting mixture was then heated to about 155° C. for 66 hours under argon. After cooling, the resulting mixture was poured into methylene chloride (400 mL) and the subsequent mixture was filtered. The filtrate was loaded on silica gel. A flash column (silica, 10% methylene chloride in hexane) and reprecipitation in methylene chloride/hexanes yielded 304 mg (42% yield) of pure product; confirmed by HNMR.

WORKUP

后处理

  1. customwas degassed for 30 minutes
  2. temperatureAfter cooling
  3. additionthe resulting mixture was poured into methylene chloride (400 mL)
  4. filtrationthe subsequent mixture was filtered
  5. customA flash column (silica, 10% methylene chloride in hexane) and reprecipitation in methylene chloride/hexanes