Bromine → Ethyl 4-(2-bromoacetyl)benzoate

HRID 650994

반응식

HRID 650994 반응식
[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]

참가 물질

6

반응물 3

HCID 24408BromineHCID 516892Sodium BicarbonateHCID 600911Ethyl 4-acetylbenzoate

생성물 1

HCID 11966043Ethyl 4-(2-bromoacetyl)benzoate수율 81.7%

시약·촉매·용매 2

HCID 6451240Aluminum(III) Chloride촉매HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e7d54fee998740bcb97886bfbd404b82
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06277873B1

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