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1-(2-Methoxy-5-trifluoromethylphenyl)ethanone → HCID 82634870、化合物

HRID 1257453
ノート
印刷プレビュー

反応式

HRID 1257453 の反応式
[CH3:1][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].[Br-:16].[Br-].[Br-].C1([N+](C)(C)C)C=CC=CC=1.C1([N+](C)(C)C)C=CC=CC=1.C1([N+](C)(C)C)C=CC=CC=1>C(OCC)C.C(=O)([O-])O.[Na+]>[Br:16][CH2:14][C:13]([C:4]1[CH:5]=[C:6]([C:9]([F:11])([F:10])[F:12])[CH:7]=[CH:8][C:3]=1[O:2][CH3:1])=[O:15]
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 99426011-(2-Methoxy-5-trifluoromethylphenyl)ethanoneHCID 17977687Phenyltrimethylammonium bromide dibromide

生成物 1

HCID 82634870HCID 82634870、化合物収率 98.8%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

To a solution of 1-[2-methoxy-5-(trifluoromethyl)phenyl]ethanone (1.00 g, 4.60 mmol) in diethyl ether (15 mL) was added phenyltrimethylammonium tribromide (1.78 g, 4.60 mmol), and the mixture was stirred overnight. The reaction mixture was diluted with diluted aqueous sodium hydrogen carbonate solution, and extracted with ethyl acetate. The extract was washed with saturated brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate) to give the title compound (1.35 g, 98%) as a colorless solid.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-c17e50be416b4ddbaca8eeeaa6bfcb0f
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461348B2

反応ノート

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