반응 #6671

반응 방정식

N,N′-diphenyl-p-phenylenediamine

iodobenzene

K2CO3

I2

→

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

수율 111.3%

용매

nitrobenzene

반응 조건

후처리

1. 1
   온도were refluxed gently over 24 hours
2. 2
   기타while removing
3. 3
   온도by reflux
4. 4
   workup.DISTILLATIONSubsequently, steam distillation
5. 5
   여과residues were filtered out
6. 6
   온도after cooling
7. 7
   세척washed with water
8. 8
   추출extracted
9. 9
   기타After removing toluene
10. 10
    workup.DISTILLATIONby distillation, ethanol
11. 11
    workup.ADDITIONwas added to the residues
12. 12
    여과the mixture was filtered
13. 13
    기타Recrystallization

실험 절차

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.

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