HRID6575

反应详情

EQUATION

反应方程式

HRID 6575 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

41.4 g of N,N′-diphenyl-p-phenylenediamine, 66 g of iodobenzene, 100 ml of nitrobenzene, 45 g of K2CO3, 10.8 g of copper powder, and I2 (trace) were put in a four-neck flask of 300-milliliter volume, and were refluxed gently over 24 hours by stirring the same while removing generated water by reflux. Subsequently, steam distillation was carried out, and when a distillate no longer came out, residues were filtered out after cooling, washed with water, and extracted using toluene. After removing toluene by distillation, ethanol was added to the residues, and the mixture was filtered. Recrystallization was carried out using a solvent of toluene and ethanol (toluene:ethanol=4:1 (by volume)), whereby 36.5 g of N,N,N′,N′-tetraphenyl-p-phenylenediamine was obtained. It had a melting point of 200° C. to 202° C.

WORKUP

后处理

  1. temperaturewere refluxed gently over 24 hours
  2. customwhile removing
  3. temperatureby reflux
  4. distillationSubsequently, steam distillation
  5. filtrationresidues were filtered out
  6. temperatureafter cooling
  7. washwashed with water
  8. extractionextracted
  9. customAfter removing toluene
  10. distillationby distillation, ethanol
  11. additionwas added to the residues
  12. filtrationthe mixture was filtered
  13. customRecrystallization