HRID719051

反应详情

EQUATION

反应方程式

HRID 719051 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
190 °C

PROCEDURE

实验过程

12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole synthesized in Example 1 (35.5 g), 4-bromobiphenyl (35.0 g), sodium bisulfite (6.0 g), a copper powder (2.4 g), 3,5-di(tert-butyl)salicylic acid (9.4 g), potassium carbonate (31.2 g), and dodecylbenzene (52 ml) were added to a nitrogen-substituted reaction vessel, heated, and stirred at 190° C. for 26 hours. After cooled to 120° C., the mixture was stirred after adding toluene (35 ml), and a crude product was collected by filtration. After adding toluene (1.6 L) to the crude product, the crude product was heated and extracted at 110° C. After cooled to a room temperature, the crude product was concentrated under reduced pressure. The product was crystallized with methanol (120 ml) to obtain a white powder of 10-(biphenyl-4-yl)-12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole (48.5 g; yield 88.1%).

WORKUP

后处理

  1. temperatureheated
  2. temperatureAfter cooled to 120° C.
  3. stirringthe mixture was stirred
  4. filtrationa crude product was collected by filtration
  5. additionAfter adding toluene (1.6 L) to the crude product
  6. temperaturethe crude product was heated
  7. extractionextracted at 110° C
  8. temperatureAfter cooled to a room temperature
  9. concentrationthe crude product was concentrated under reduced pressure
  10. customThe product was crystallized with methanol (120 ml)