反応 #1605812

ord-c1a270181535486187596470ab6be54a

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The solution was concentrated under reduced pressure, to the residue
  2. 2
    workup.ADDITIONwas added water (20 mL) and subsequently ethanol (30 mL)
  3. 3
    workup.STIRRINGthe mixture was stirred under ice bath for 1 hour
  4. 4
    ろ過The precipitate was collected by filtration
  5. 5
    洗浄washed with ethanol/water (=1:1)
  6. 6
    その他dried under reduced pressure

実験手順

2-Phenyl-N-acetylaniline (6.21 g, 29.40 mmol) was dissolved in acetic acid (70 mL). Thereto was dropwise added under ice bath a separately prepared solution of hydrogen bromide (6.14 g, 38.42 mmol) dissolved in carbon tetrachloride (19.21 mL) and the mixture was stirred at room temperature overnight. The solution was concentrated under reduced pressure, to the residue was added water (20 mL) and subsequently ethanol (30 mL), and the mixture was stirred under ice bath for 1 hour. The precipitate was collected by filtration, washed with ethanol/water (=1:1), dried under reduced pressure to obtain 2-phenyl-4-bromo-N-acetylaniline (7.79 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09072734B2uspto-grants-2015_07