HRID532317

反应详情

EQUATION

反应方程式

HRID 532317 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

2-Bromo-9,9-dimethyl-7,10-diphenylacridan (3.2 g), (biphenyl-4-yl)-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaboran-2-yl)phenyl]-phenylamine (3.6 g), toluene (40 ml), ethanol (10 ml), and a 2M potassium carbonate aqueous solution (11 ml) were added to a nitrogen-substituted reaction vessel and aerated with nitrogen gas for 30 min under ultrasonic irradiation. The mixture was heated after adding tetrakis(triphenylphosphine)palladium (0.26 g) and stirred at 72° C. for 7 hours. The mixture was allowed to cool to a room temperature, and methanol (50 ml) was added. A precipitated solid was collected by filtration and washed with water to obtain a red brown crude product. The crude product was dissolved by adding toluene (100 ml) and subjected to adsorptive purification twice using silica gel (3.7 g). The product was then crystallized with toluene/methanol to obtain a white powder of (biphenyl-4-yl)-[4-(9,9-dimethyl-7,10-diphenylacridan-2-yl)phenyl]-phenylamine (3.42 g; yield 68%).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto cool to a room temperature
  3. filtrationA precipitated solid was collected by filtration
  4. washwashed with water
  5. customto obtain a red brown crude product
  6. custompurification twice using silica gel (3.7 g)
  7. customThe product was then crystallized with toluene/methanol