反応 #1605813

ord-2d5602354ea84c34b8c1ca9d286ce53d

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture was heated
  2. 2
    温度under reflux overnight
  3. 3
    濃縮The solution was concentrated under reduced pressure and to the residue
  4. 4
    workup.ADDITIONwere added ethyl acetate (50 mL) and water (40 mL)
  5. 5
    抽出for extraction
  6. 6
    乾燥The organic layer was dried over sodium sulfate
  7. 7
    ろ過after filtration
  8. 8
    濃縮concentrated under reduced pressure
  9. 9
    その他The residue was purified by a silica gel column

実験手順

2-Phenyl-4-bromo-N-acetylaniline (7.79 g, 26.85 mmol) was dissolved in ethanol (100 mL), 2 N hydrochloric acid (33.56 mmol, 67.12 mL) was added dropwise under ice bath, and the mixture was heated under reflux overnight. The solution was concentrated under reduced pressure and to the residue were added ethyl acetate (50 mL) and water (40 mL) for extraction. The organic layer was dried over sodium sulfate and, after filtration, concentrated under reduced pressure. The residue was purified by a silica gel column to obtain 2-phenyl-4-bromoaniline (6.58 g).

出典

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