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Tetra-n-butylammonium tribromide → HCID 58442377、化合物

HRID 1465606
ノート
印刷プレビュー

反応式

HRID 1465606 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([C:9](=[O:11])[CH3:10])=[C:4]([CH3:12])[CH:3]=1.[Br-:13].[Br-].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC>C(#N)C>[Br:13][CH2:10][C:9]([C:5]1[C:4]([CH3:12])=[CH:3][C:2]([Cl:1])=[CH:7][C:6]=1[CH3:8])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 23500184Tetra-n-butylammonium tribromideHCID 534028641-(4-chloro-2,6-dimethylphenyl)ethanone

生成物 1

HCID 58442377HCID 58442377、化合物収率 102%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 1-(4-chloro-2,6-dimethylphenyl)ethanone (5.0 g, 27 mmol) in acetonitrile (54.8 mL) was added tetrabutylammoniumtribromide (TBABr3, 13.2 g, 27.4 mmol). The reaction was stirred at room temperature overnight. The solution was concentrated under reduced pressure, added with water, and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous MgSO4(s), and concentrated under reduced pressure to give 2-bromo-1-(4-chloro-2,6-dimethylphenyl)ethanone (7.2 g), which was used directly for the next step without further purification.

後処理

  1. concentrationThe solution was concentrated under reduced pressure
  2. additionadded with water
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous MgSO4(s)
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b2a7fc0116a245b6a9a00cdc3157855d
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08999983B2

反応ノート

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