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4-Iodoanisole → N-([1,1'-biphenyl]-4-yl)-N-(4-methoxyphenyl)-[1,1':3',1''-terphenyl]-4'-amine

HRID 1021177
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HRID 1021177 반응식
P(C(C)(C)C)(C(C)(C)C)C(C)(C)C.[C:14]1([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)[CH:19]=[CH:18][C:17]([NH:20][C:21]2[CH:26]=[CH:25][C:24]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[CH:23][C:22]=2[C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[CH:16][CH:15]=1.I[C:46]1[CH:51]=[CH:50][C:49]([O:52][CH3:53])=[CH:48][CH:47]=1.CC(C)([O-])C.[Na+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].CCCCCC>[C:14]1([C:39]2[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=2)[CH:19]=[CH:18][C:17]([N:20]([C:46]2[CH:51]=[CH:50][C:49]([O:52][CH3:53])=[CH:48][CH:47]=2)[C:21]2[CH:26]=[CH:25][C:24]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[CH:23][C:22]=2[C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 696764-IodoanisoleHCID 83681Tris(1,1-dimethylethyl)phosphineHCID 23676156Sodium t-butoxideHCID 86762383N-([1,1'-biphenyl]-4-yl)-[1,1':3',1''-terphenyl]-4'-amine

생성물 1

HCID 86762390N-([1,1'-biphenyl]-4-yl)-N-(4-methoxyphenyl)-[1,1':3',1''-terphenyl]-4'-amine수율 94%

시약·촉매·용매 2

HCID 8058
Hexane
촉매
HCID 9811564Bis(dibenzylideneacetone)palladium촉매

실험 절차

Toluene (200 mL) was bubbled with nitrogen for 15 min, followed by addition of 10% t-Bu3P in hexane (2.9 mL, 1.0 mmol) and Pd2(dba)3 (1.1 g, 1.2 mmol). The mixture was bubbled with nitrogen for 15 min, then N-([1,1′-biphenyl]-4-yl)-[1,1′:3′,1″-terphenyl]-4′-amine (10.6 g, 26.5 mmol), 4-iodoanisole (11.2 g, 48.0 mmol), sodium tert-butoxide (3.5 g, 36.0 mmol) were added. The mixture was bubbled with nitrogen for 15 min and stirred for 16 h at room temperature. The reaction mixture was filtered through a silica pad and washed with toluene (containing 0.5% triethylamine). The solvent was removed in vacuo and the residue was purified by flash chromatography using 30-40% toluene/hexane (containing 0.5% triethylamine) to afford N-([1,1′-biphenyl]-4-yl)-N-(4-methoxyphenyl)-[1,1′:3′,1″-terphenyl]-4′-amine (12.5 g, 94% yield) as a white solid.

후처리

  1. customToluene (200 mL) was bubbled with nitrogen for 15 min
  2. customThe mixture was bubbled with nitrogen for 15 min
  3. customThe mixture was bubbled with nitrogen for 15 min
  4. filtrationThe reaction mixture was filtered through a silica pad
  5. washwashed with toluene (containing 0.5% triethylamine)
  6. customThe solvent was removed in vacuo
  7. customthe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-2f8558c126e34378bcd9258097a7ffb4
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716484B1

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