HRID555929

反应详情

EQUATION

反应方程式

HRID 555929 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A degassed solution of 489.5 mg (0.156%) of copper(I) chloride and 906 mg (1%) mmol) of 1,10-phenanthroline in 100 ml of toluene were saturated with N2 for 1 hour and heated to 130° C. The solution was subsequently admixed with 16.2 g (50 mmol) of 2,7-dibromocarbazole and 13.2 g (50 mmol) of 1-iodo-4-tert-butylbenzene and heated at 180° C. for 2 hours. After cooling, the mixture was admixed with 180 ml of water, the organic phase was separated off and the solvent was removed under reduced pressure. The product was recrystallized from n-hexane. Yield: 13 g (59%). Purity according to HPLC: 99.5%

WORKUP

后处理

  1. temperatureheated at 180° C. for 2 hours
  2. temperatureAfter cooling
  3. customthe organic phase was separated off
  4. customthe solvent was removed under reduced pressure
  5. customThe product was recrystallized from n-hexane