HRID1670167

反应详情

EQUATION

反应方程式

HRID 1670167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-bromo triphenylamine 7.6 g (23.45 mmol), aniline 21.85 g (0.235 mol), sodium tert-butoxide 6.76 g (70 mmol). Pd2(dba)3[(tris(dibenzilidene acetone)dipalladium(0))] 0.86 g (0.938 mmol) and tri(tert-butyl)phosphine 0.23 g (1.173 mmol) in 500 ml round bottom flask were dissolved with toluene 200 ml, and refluxed for 12 hours. After the reaction was terminated, the reaction solution was cooled to room temperature, and 200 ml of distilled water was added thereto to extract an organic layer. The organic layer was dried over MgSO4, concentrated, and purified by silica gel column chromatography. The eluate was concentrated and dried to give N,N,N′-triphenyl-p-phenylenediamine (6.71 g, 85%).

WORKUP

后处理

  1. temperaturerefluxed for 12 hours
  2. customAfter the reaction was terminated
  3. addition200 ml of distilled water was added
  4. extractionto extract an organic layer
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated
  7. custompurified by silica gel column chromatography
  8. concentrationThe eluate was concentrated
  9. customdried