تفاعل #6671

معادلة التفاعل

N,N′-diphenyl-p-phenylenediamine

iodobenzene

K2CO3

I2

→

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

المردود 111.3%

المذيبات

nitrobenzene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwere refluxed gently over 24 hours
2. 2
   أخرىwhile removing
3. 3
   درجة الحرارةby reflux
4. 4
   workup.DISTILLATIONSubsequently, steam distillation
5. 5
   ترشيحresidues were filtered out
6. 6
   درجة الحرارةafter cooling
7. 7
   غسيلwashed with water
8. 8
   استخلاصextracted
9. 9
   أخرىAfter removing toluene
10. 10
    workup.DISTILLATIONby distillation, ethanol
11. 11
    workup.ADDITIONwas added to the residues
12. 12
    ترشيحthe mixture was filtered
13. 13
    أخرىRecrystallization

الإجراء التجريبي

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.

المصدر