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Boron tribromide → 1-(2-Hydroxy-5-(trifluoromethyl)phenyl)ethan-1-one

HRID 46381
ノート
印刷プレビュー

反応式

HRID 46381 の反応式
C[O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][C:4]=1[C:13](=[O:15])[CH3:14].B(Br)(Br)Br>ClCCl.[I-].C([N+](CCCC)(CCCC)CCCC)CCC>[OH:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:10])([F:11])[F:12])=[CH:5][C:4]=1[C:13](=[O:15])[CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 25134Boron tribromideHCID 99426011-(2-Methoxy-5-trifluoromethylphenyl)ethanone

生成物 1

HCID 117695991-(2-Hydroxy-5-(trifluoromethyl)phenyl)ethan-1-one収率 35.2%

試薬・触媒・溶媒 2

HCID 67553Tetrabutylammonium Iodide触媒HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 1-[2-methoxy-5-(trifluoromethyl)phenyl]ethanone (35 g, 0.160 mol) in dry dichloromethane (400 mL) at 0° C. was added solid tetrabutylammonium iodide (2.96 g, 0.008 mol) followed by boron tribromide (33.96 mL, 0.353 mol) dropwise. After addition, the reaction mixture was stirred at room temperature for 90 minutes. The reaction mixture was cooled to 0° C. and quenched with ice. The mixture was extracted with diethyl ether (1000 mL). The organic layer was washed with water (2000 mL) and then saturated aqueous sodium chloride (1000 mL). After concentration of the organic layer at room temperature in vacuo, the crude product was purified by column chromatography (100-200 silica gel, 2% v/v diethyl ether in hexane) to give 11.5 g (35%) of the title compound as a colourless oil.

後処理

  1. additionAfter addition
  2. temperatureThe reaction mixture was cooled to 0° C.
  3. customquenched with ice
  4. extractionThe mixture was extracted with diethyl ether (1000 mL)
  5. washThe organic layer was washed with water (2000 mL)
  6. customAfter concentration of the organic layer at room temperature in vacuo, the crude product was purified by column chromatography (100-200 silica gel, 2% v/v diethyl ether in hexane)

出典と根拠

ORDレコード
ord-70b6a9696d13437a87ea73275552b049
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08541588B2

反応ノート

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