HRID1037509

反应详情

EQUATION

反应方程式

HRID 1037509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1,3-diiodobenzene (50.0 g, 0.152 mol), carbazole (55.0 g, 0.329 mol), Cu (40.0 g, 0.630 mol) and 18-crown-6 (0.5 g) in 1,2-dichlorobenzene (200.0 ml) was added potassium carbonate (150.0 g, 1.085 mol) under nitrogen and stirring. The reaction was carried out at 190° C. for 12 hours. After cooling, the reaction mixture was filtrated. The solid residues were carefully washed with THF. Then, THF and 1,2-dichlorobenzene were evaporated from the combined filtration solution. The crude product was purified by recrystallization from acetone/methanol to give 47.0 g (75.7%) in yield.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture was filtrated
  3. washThe solid residues were carefully washed with THF
  4. customThen, THF and 1,2-dichlorobenzene were evaporated from the combined filtration solution
  5. customThe crude product was purified by recrystallization from acetone/methanol
  6. customto give 47.0 g (75.7%)
  7. customin yield