반응 #812913

반응 방정식

N-phenyl-p-normalbutylaniline

4,4'-diiodobiphenyl

potassium carbonate

→

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

수율 58.7%

반응 조건

후처리

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

실험 절차

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.

출처