HRID929284

反应详情

EQUATION

反应方程式

HRID 929284 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Indolo[3,2-b]carbazole (1.20 g, 4,68 mmol) was suspended in 48 ml of o-xylene under nitrogen and treated with iodobenzene (2.10 g, 10.3 mmol) followed by the sodium t-butoxide (1.35 g, 14.0 mmol), tri-t-butylphosphine (0.15 g, 0.74 mmol) and palladium dibenzylideneacetone (0.34 g, 0.37 mmol). The resulting mixture was heated to 120° C. and stirred for 20 minutes. It was then cooled to room temperature filtered through a short pad of silica gel and the pad washed with toluene. The combined filtrates were combined and concentrated to dryness to afford a dark-colored solid. Purification using a Biotage® automated flash purification system afforded 0.640 g of N,N′-bis(phenyl)-indolo[3,2-b]carbazole with a purity of 99.7%. MP=306.5° C.; Tg=238.9° C.

WORKUP

后处理

  1. temperatureIt was then cooled to room temperature
  2. filtrationfiltered through a short pad of silica gel
  3. washthe pad washed with toluene
  4. concentrationconcentrated to dryness
  5. customto afford a dark-colored solid
  6. customPurification
  7. customflash purification system