Aniline → N4,N4,N4'-Triphenyl-[1,1'-biphenyl]-4,4'-diamine

HRID 31954

반응식

HRID 31954 반응식
C(P(C(C)(C)C)C(C)(C)C)(C)(C)C.Br[C:15]1[CH:20]=[CH:19][C:18]([C:21]2[CH:26]=[CH:25][C:24]([N:27]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)=[CH:23][CH:22]=2)=[CH:17][CH:16]=1.[NH2:40][C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1.C(O[Na])(C)(C)C>C1(C)C=CC=CC=1>[C:28]1([N:27]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[C:24]2[CH:25]=[CH:26][C:21]([C:18]3[CH:19]=[CH:20][C:15]([NH:40][C:41]4[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=4)=[CH:16][CH:17]=3)=[CH:22][CH:23]=2)[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

참가 물질

6

반응물 4

HCID 6115AnilineHCID 83681Tris(1,1-dimethylethyl)phosphineHCID 113155504-Bromo-4'-(diphenylamino)biphenylHCID 178418730sodium 2-methylpropan-2-olate

생성물 1

HCID 22013295N4,N4,N4'-Triphenyl-[1,1'-biphenyl]-4,4'-diamine수율 77.6%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

A 0.66 weight % toluene solution 100 μl of tri-t-butylphosphine was added to a toluene 100 ml solution of 4-bromo-4′-(N,N-diphenylamino)biphenyl 4.00 g, aniline 1.11 g, tris(benzylideneacetone)-dipalladium (0) 183 mg and t-butoxysodium 1.35 g, and the mixture was stirred at room temperature for 5 hours. After finishing the reaction, the mixture was filtered through celite, and the filtrate was extracted with toluene. This was concentrated under reduced pressure, and the resulting crude product was subjected to column refining to obtain 3.20 g of pale yellow powder of N,N,N′-triphenylbenzidine.

후처리

  1. customthe reaction
  2. filtrationthe mixture was filtered through celite
  3. extractionthe filtrate was extracted with toluene
  4. concentrationThis was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e0f170690ca544d8bc6d4dc7f67f0364
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425654B2

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