HRID1753711

反应详情

EQUATION

反应方程式

HRID 1753711 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of 10.9 g (35.1 mmol) 4-iododibenzo[b,d]thiophene, 8.6 g (35.1 mmol) of 3-bromo-9H-carbazole, 4.46 g (70.2 mmol) of Cu, 14.55 g (100.1 mmole) of K2CO3 was stirred in 100 ml dimethylformamide, the reaction mixture was then heat to 160° C. for about overnight under nitrogen. Then cooled to 100° C., the solution was filtered. To receive the filtrate, and most of the dimethylformamide was removed under reduced pressure from the filtrate. The distillation was extracted with ethyl acetate and water, dried with anhydrous magnesium sulfate, the solvent was removed and the residue was purified by column chromatography on silica(hexane-dichloromethane) to give product 8.7 g (58%).

WORKUP

后处理

  1. temperatureThen cooled to 100° C.
  2. filtrationthe solution was filtered
  3. custommost of the dimethylformamide was removed under reduced pressure from the filtrate
  4. distillationThe distillation
  5. extractionwas extracted with ethyl acetate and water
  6. dry with materialdried with anhydrous magnesium sulfate
  7. customthe solvent was removed
  8. customthe residue was purified by column chromatography on silica(hexane-dichloromethane)