反応 #6671

反応方程式

N,N′-diphenyl-p-phenylenediamine

iodobenzene

K2CO3

I2

→

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

収率 111.3%

溶媒

nitrobenzene

反応条件

後処理

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

実験手順

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.

出典