HRID481935

反应详情

EQUATION

反应方程式

HRID 481935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 500-ml reactor was charged with 33.6 g (0.10 mol) of N,N'-diphenylbenzidine, 25.0 g (0.11 mol) of m-iodotoluene, 27.6 g (0.2 mol) of potassium carbonate, 2.6 g of copper powder, and 200 ml of nitrobenzene. In an argon stream, the contents were heated under reflux for 24 hours. At the end of reaction, the insoluble was removed by filtration and the solvent was distilled off from the filtrate. The still residue was purified twice through a silica gel column with a 1/2mixture of n-hexane and toluene, obtaining 28.10 g of N,N'-diphenyl-N-[4-(N-phenyl-N-3-methylphenylamino)-biphenyl-4-yl]benzidine (yield 42%).

WORKUP

后处理

  1. temperatureIn an argon stream, the contents were heated
  2. temperatureunder reflux for 24 hours
  3. customAt the end of reaction
  4. customthe insoluble was removed by filtration
  5. distillationthe solvent was distilled off from the filtrate
  6. customThe still residue was purified twice through a silica gel column with a 1/2mixture of n-hexane and toluene