Bromine → Ethyl 4-(2-bromoacetyl)benzoate

HRID 650994

反応式

HRID 650994 の反応式
[C:1]([C:4]1[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[Br:15]Br.C([O-])(O)=O.[Na+]>CCOCC.[Cl-].[Al+3].[Cl-].[Cl-]>[Br:15][CH2:2][C:1]([C:4]1[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=1)=[O:3]

参加物

6

反応物 3

HCID 24408BromineHCID 516892Sodium BicarbonateHCID 600911Ethyl 4-acetylbenzoate

生成物 1

HCID 11966043Ethyl 4-(2-bromoacetyl)benzoate収率 81.7%

試薬・触媒・溶媒 2

HCID 6451240Aluminum(III) Chloride触媒HCID 3283Diethyl Ether溶媒

実験手順

To a solution of ethyl 4-acetylbenzoate (5.12 g, 26.6 mmol) in ether (50 ml) containing aluminium chloride (0.025 g, 0.19 mmol) is added bromine (1.31 ml, 26.6 mmol) and the reaction mixture is stirred for 2 h. The reaction mixture is poured into saturated NaHCO3 solution and stirred for 30 min. and the layers are separated. The organic layer is washed with NaHCO3, H2O, dried over MgSO4, concentrated to half of its volume and refrigerated overnight. The resulting solid is filtered to yield ethyl 4-(2′-bromoacetyl)benzoate (5.89 g, 81.6%) as white crystals.

後処理

  1. stirringstirred for 30 min.
  2. customthe layers are separated
  3. washThe organic layer is washed with NaHCO3, H2O
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated to half of its volume and refrigerated overnight
  6. filtrationThe resulting solid is filtered

出典と根拠

ORDレコード
ord-e7d54fee998740bcb97886bfbd404b82
出典データセット
uspto-grants-2001_08
特許番号
US06277873B1

関連ノート

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