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Benzene → 2'-Trifluoromethyl-biphenyl-4-ylamine

HRID 1062658
ノート
印刷プレビュー

反応式

HRID 1062658 の反応式
Br[C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][CH:3]=1.[F:9][C:10]([F:21])([F:20])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1B(O)O.C(=O)([O-])[O-].[Na+].[Na+].C1C=CC=CC=1>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C(Cl)Cl.O.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[NH2:6][C:5]1[CH:7]=[CH:8][C:2]([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[C:10]([F:21])([F:20])[F:9])=[CH:3][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 241BenzeneHCID 78074-BromoanilineHCID 10340Sodium CarbonateHCID 27343872-(Trifluoromethyl)benzeneboronic acid

生成物 1

HCID 27607432'-Trifluoromethyl-biphenyl-4-ylamine収率 44.1%

試薬・触媒・溶媒 4

HCID 74236Tetrabutylammonium Bromide
触媒
HCID 11979704Tetrakis(triphenylphosphine)palladium触媒
HCID 962Water溶媒
HCID 6344Dichloromethane溶媒

実験手順

A mixture of 3.44 g (20 mmol) of 4-bromoaniline and 3.80 g (20 mmol) of 2-(trifluoromethyl)phenylboronic acid, 1.16 g of tetrakis(triphenylphosphine) palladium(0) (1 mmol), 0.32 g of tetrabutylammonium bromide (1 mmol) and 20 mL of 2M aqueous sodium carbonate were refluxed with 180 mL of benzene under N2 for 14 hours. After cooling, the mixture was diluted with methylene chloride and water. The two phases were separated and the organic phase was washed with water, dried with MgSO4 and concentrated in vacuo. The resulting thick oil was chromatographed on silica with 10% EtOAc/hexane to afford 2.09 g (44%) of the aniline. 1H NMR (CDCl3) δ: 7.72 (d, 1H); 7.53 (t, 1H); 7.41 (t, 1H); 7.32 (d, 1H); 7.13 (d, 2H); 6.73 (d, 2H); 3.74 (br s, 2H).

後処理

  1. temperatureAfter cooling
  2. customThe two phases were separated
  3. washthe organic phase was washed with water
  4. dry with materialdried with MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe resulting thick oil was chromatographed on silica with 10% EtOAc/hexane

出典と根拠

ORDレコード
ord-b9e435c589424f25a57dc694b27f6c90
出典データセット
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06962935B2

反応ノート

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