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Carbazole → 9-(3'-bromo-[1,1'-biphenyl]-3-yl)-9H-carbazole

HRID 1424767
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HRID 1424767 반응식
[CH:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[Br:14][C:15]1[CH:16]=[C:17]([C:21]2[CH:26]=[CH:25][CH:24]=[C:23](Br)[CH:22]=2)[CH:18]=[CH:19][CH:20]=1.CC([O-])(C)C.[Na+]>C1(C)C(C)=CC=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.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(P(C2C=CC=CC=2)[C-]2C=CC=C2)C=CC=CC=1.[C-]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C1.[Fe+2]>[Br:14][C:15]1[CH:16]=[C:17]([C:21]2[CH:22]=[CH:23][CH:24]=[C:25]([N:12]3[C:11]4[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=4[C:5]4[C:13]3=[CH:1][CH:2]=[CH:3][CH:4]=4)[CH:26]=2)[CH:18]=[CH:19][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 6854CarbazoleHCID 1539873,3'-DibromobiphenylHCID 23676156Sodium t-butoxide

생성물 1

HCID 588711539-(3'-bromo-[1,1'-biphenyl]-3-yl)-9H-carbazole수율 54.7%

시약·촉매·용매 3

HCID 635956Ferrocene-1,1'-bis-(diphenylphosphine)촉매
HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 7237O-Xylene용매

실험 절차

9H-carbazole (10 g, 59.8 mmol) and 3,3′-dibromo-1,1′-biphenyl (41.1 g, 132 mmol) were dissolved in xylene (100 ml). Sodium 2-methylpropan-2-olate (8.62 g, 90 mmol), Tris(dibenzylideneacetone)dipalladium(0) (Pd2dba3) (0.548 g, 0.598 mmol) and 1,1′-bis(diphenylphosphanyl) ferrocene (dppf) (0.663 g, 1.196 mmol) were then added into the mixture. The reaction mixture was degassed with nitrogen for 30 minutes, and heated to reflux for 48 h. The crude mixture was filtered through a pad of Celite® and washed with DCM. The solvents were evaporated under vacuum and the material was purified via column chromatography using hexane and DCM (95/5). After the excess of dibromobiphenyl came out, the polarity was increased gradually to 30% DCM in hexane. The compound 9-(3′-bromo-[1,1′-biphenyl]-3-yl)-9H-carbazole (13.02 g, 32.7 mmol, 54.7% yield) was afforded as white solids.

후처리

  1. customThe reaction mixture was degassed with nitrogen for 30 minutes
  2. temperatureheated
  3. temperatureto reflux for 48 h
  4. filtrationThe crude mixture was filtered through a pad of Celite®
  5. washwashed with DCM
  6. customThe solvents were evaporated under vacuum
  7. customthe material was purified via column chromatography
  8. temperaturethe polarity was increased gradually to 30% DCM in hexane

출처 및 근거

ORD 기록
ord-cabf28ecc2e94ed8bbc28e6a0aceb5ad
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08927749B2

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