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

HRID 337392
ノート
印刷プレビュー

反応式

HRID 337392 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

反応条件

温度
180 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1fcb01bcd9814ae29c81c42c04007f39
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08889726B2

反応ノート

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