反应 #6671

反应方程式

N,N′-diphenyl-p-phenylenediamine

iodobenzene

K2CO3

I2

→

N,N,N′,N′-tetraphenyl-p-phenylenediamine

收率 111.3%

溶剂

nitrobenzene

反应条件

后处理

1. 1
   温度were refluxed gently over 24 hours
2. 2
   其他while removing
3. 3
   温度by reflux
4. 4
   workup.DISTILLATIONSubsequently, steam distillation
5. 5
   过滤residues were filtered out
6. 6
   温度after cooling
7. 7
   洗涤washed with water
8. 8
   萃取extracted
9. 9
   其他After removing toluene
10. 10
    workup.DISTILLATIONby distillation, ethanol
11. 11
    workup.ADDITIONwas added to the residues
12. 12
    过滤the mixture was filtered
13. 13
    其他Recrystallization

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.

来源