HRID625200

反应详情

EQUATION

反应方程式

HRID 625200 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
72 °C

PROCEDURE

实验过程

The resulting 9-(4-bromophenyl)-9′-phenyl-9H,9′H-[3,3′]bicarbazolyl (17.00 g), 9-phenyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxabororan-2-yl)-9H-carbazole (12.25 g), toluene (160 ml), ethanol (40 ml), and a 2 M potassium carbonate aqueous solution (23 ml) were added to a nitrogen-substituted reaction vessel, and aerated with nitrogen gas for 30 minutes under ultrasonic waves. After adding tetrakis(triphenylphosphine)palladium (1.74 g), the mixture was heated, and stirred at 72° C. for 12.5 hours. The mixture was allowed to cool to room temperature, and extraction was performed by adding toluene (100 ml) and water (150 ml) thereto. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure to obtain a black crude product. The crude product was purified by column chromatography (carrier: silica gel; eluent: hexane/toluene) to obtain a pale yellowish white powder of 9′-phenyl-9-[4-(9-phenyl-9H-carbazol-3-yl)-phenyl]-9H,9′H-[3,3′]bicarbazolyl (10.44 g; yield 48%).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto cool to room temperature
  3. extractionextraction
  4. additionby adding toluene (100 ml) and water (150 ml)
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customto obtain a black crude product
  8. customThe crude product was purified by column chromatography (carrier: silica gel; eluent: hexane/toluene)