3-Methylacetophenone → 1-(3-(Bromomethyl)phenyl)ethan-1-one

HRID 1356777

反応式

HRID 1356777 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([C:8](=[O:10])[CH3:9])[CH:5]=[CH:6][CH:7]=1.[Br:11]N1C(=O)CCC1=O>C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.C(Cl)(Cl)(Cl)Cl>[Br:11][CH2:1][C:2]1[CH:3]=[C:4]([C:8](=[O:10])[CH3:9])[CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 114553-MethylacetophenoneHCID 67184N-bromobutanimide

生成物 1

HCID 154798071-(3-(Bromomethyl)phenyl)ethan-1-one収率 38.8%

試薬・触媒・溶媒 2

HCID 7187Benzoyl Peroxide触媒HCID 5943Carbon Tetrachloride溶媒

実験手順

3′-Methylacetophenone (5.00 g; 37.3 mmol), N-bromosuccinimide (6.63 g; 37.3 mmol), and benzoyl peroxide (100 mg) were added to carbon tetrachloride (70 ml), and the mixture was refluxed for 1 hour. The mixture was left to cool to room temperature, and crystals that precipitated were removed by filtration. The filtrate was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1), to thereby yield 3.08 g of the target compound (yield: 38.8%).

後処理

  1. temperaturethe mixture was refluxed for 1 hour
  2. waitThe mixture was left
  3. customcrystals that precipitated
  4. customwere removed by filtration
  5. customThe filtrate was evaporated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1)

出典と根拠

ORDレコード
ord-fabc5a7317ba403681b8e1ab8e4315af
出典データセット
uspto-grants-2003_07
特許番号
US06586633B1

関連ノート

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