HRID1485597

反应详情

EQUATION

反应方程式

HRID 1485597 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

A degassed solution of 157.6 g (400 mmol) of diethyl dibromoterephthalate and 36.7 g (220 mmol) of carbazole in 1 l of 1,2-dichlorobenzene is saturated with N2 for 1 h. Then, firstly 20 g (314 mmol) of copper powder, then 18 g (67 mmol) of 18-crown-6 are added to the solution, and 177 g (850 mmol) of potassium carbonate as the solid are subsequently added. The reaction mixture is heated at 170° C. for 18 h. After cooling to room temperature, 1 l of water is carefully added. The organic phase is washed with 4×50 ml of H2O and dried over MgSO4, and the solvents are removed in vacuo. The pure product is obtained by recrystallisation. The yield is 83 g (177 mmol), corresponding to 81% of theory.

WORKUP

后处理

  1. additionare subsequently added
  2. temperatureAfter cooling to room temperature
  3. washThe organic phase is washed with 4×50 ml of H2O
  4. dry with materialdried over MgSO4
  5. customthe solvents are removed in vacuo
  6. customThe pure product is obtained by recrystallisation