تفاعل #812913

معادلة التفاعل

N-phenyl-p-normalbutylaniline

4,4'-diiodobiphenyl

potassium carbonate

→

N,N'-bis(p-normalbutylphenyl)-N,N'-diphenylbenzidine

المردود 58.7%

ظروف التفاعل

المعالجة

1. 1
   أخرىreaction at a temperature of 170° to 220° C. for 27 hours
2. 2
   استخلاصThe reaction product was then extracted with 140 ml of toluene
3. 3
   أخرىThe insoluble contents were removed by filtration
4. 4
   تركيزThe filtrate was then concentrated
5. 5
   أخرىto obtain an oily material
6. 6
   أخرىThe crude product thus obtained
7. 7
   أخرىwas then purified by column chromatography (carrier: silica gel; elute: 1/5 mixture of toluene and n-hexane)

الإجراء التجريبي

21.1 g (0.094 mol) of N-phenyl-p-normalbutylaniline, 15.4 g (0.038 mol) of 4,4'-diiodobiphenyl, 15.7 g (0.11 mol) of anhydrous potassium carbonate, and 1.1 g (0.017 mol) of copper powder were mixed. The mixture was then allowed to undergo reaction at a temperature of 170° to 220° C. for 27 hours. The reaction product was then extracted with 140 ml of toluene. The insoluble contents were removed by filtration. The filtrate was then concentrated to obtain an oily material. The crude product thus obtained was then purified by column chromatography (carrier: silica gel; elute: 1/5 mixture of toluene and n-hexane) to obtain 13.4 g (yield: 58.6%) of N,N'-bis(p-normalbutylphenyl)-N,N'-diphenylbenzidine. The melting point of the product was from 135.0° C. to 135.5° C.

المصدر