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Hexane → 1-(7-acetyl-9H-carbazol-2-yl)ethanone

HRID 337392
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HRID 337392 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[N+:20]([C:23]1[CH:28]=[C:27]([C:29](=[O:31])[CH3:30])[CH:26]=[CH:25][C:24]=1[C:32]1[CH:37]=[CH:36][C:35]([C:38](=[O:40])[CH3:39])=[CH:34][CH:33]=1)([O-])=O.CCCCCC>ClC1C=CC=CC=1Cl>[CH:36]1[C:37]2[NH:20][C:23]3[C:24](=[CH:25][CH:26]=[C:27]([C:29](=[O:31])[CH3:30])[CH:28]=3)[C:32]=2[CH:33]=[CH:34][C:35]=1[C:38](=[O:40])[CH3:39]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8058HexaneHCID 11776TriphenylphosphineHCID 712724381,1'-(2-Nitro-[1,1'-biphenyl]-4,4'-diyl)diethanone

생성물 1

HCID 42891861-(7-acetyl-9H-carbazol-2-yl)ethanone

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

반응 조건

온도
180 °C

실험 절차

The mixture of triphenylphosphine (3.47 g, 13.24 mmol) and 1,1′-(2-nitro-[1,1′-biphenyl]-4,4′-diyl)diethanone (1.5 g, 5.30 mmol) in 1,2-dichlorobenzene (o-DCB) (15.90 mL) was heated at 180° C. under microwave irradiation for 1 h. The reaction mixture was cooled and poured in to the hexane (50 mL). Most of the impurities were removed by precipitation from hexane. The compound was further purified on silica gel ((0-100% EtOAc/Hexane). Fractions were concentrated to give the title compound as a yellow solid.

후처리

  1. temperatureThe reaction mixture was cooled
  2. customMost of the impurities were removed by precipitation from hexane
  3. customThe compound was further purified on silica gel ((0-100% EtOAc/Hexane)
  4. concentrationFractions were concentrated

출처 및 근거

ORD 기록
ord-1fcb01bcd9814ae29c81c42c04007f39
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08889726B2

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