반응식
[C:1]1([NH:7][C:8]2[CH:13]=[CH:12][C:11]([C:14]3[CH:26]=[CH:25][C:17]([NH:18][C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)=[CH:16][CH:15]=3)=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.I[C:28]1[CH:29]=[C:30]([CH3:34])[CH:31]=[CH:32][CH:33]=1.C(=O)([O-])[O-].[K+].[K+]>[Cu].[N+](C1C=CC=CC=1)([O-])=O>[C:19]1([N:18]([C:33]2([N:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[C:28]3[CH:33]=[CH:32][CH:31]=[C:30]([CH3:34])[CH:29]=3)[CH:32]=[CH:31][C:30]([C:34]3[CH:10]=[CH:9][CH:8]=[CH:13][CH:12]=3)=[CH:29][CH2:28]2)[C:17]2[CH:25]=[CH:26][C:14]([C:11]3[CH:12]=[CH:13][C:8]([NH:7][C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)=[CH:9][CH:10]=3)=[CH:15][CH:16]=2)[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1참가 물질
6
실험 절차
A 500-ml reactor was charged with 33.6 g (0.10 mol) of N,N'-diphenylbenzidine, 25.0 g (0.11 mol) of m-iodotoluene, 27.6 g (0.2 mol) of potassium carbonate, 2.6 g of copper powder, and 200 ml of nitrobenzene. In an argon stream, the contents were heated under reflux for 24 hours. At the end of reaction, the insoluble was removed by filtration and the solvent was distilled off from the filtrate. The still residue was purified twice through a silica gel column with a 1/2mixture of n-hexane and toluene, obtaining 28.10 g of N,N'-diphenyl-N-[4-(N-phenyl-N-3-methylphenylamino)-biphenyl-4-yl]benzidine (yield 42%).
후처리
- temperatureIn an argon stream, the contents were heated
- temperatureunder reflux for 24 hours
- customAt the end of reaction
- customthe insoluble was removed by filtration
- distillationthe solvent was distilled off from the filtrate
- customThe still residue was purified twice through a silica gel column with a 1/2mixture of n-hexane and toluene
출처 및 근거
- ORD 기록
- ord-f5a2a4faecb346f3b3a380bb69592689
- 출처 데이터셋
- uspto-grants-1998_08
- 특허 번호
- US05792557
연결된 노트
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