Réaction #1605813

ord-2d5602354ea84c34b8c1ca9d286ce53d

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurethe mixture was heated
  2. 2
    Températureunder reflux overnight
  3. 3
    ConcentrationThe 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
    Extractionfor extraction
  6. 6
    SéchageThe organic layer was dried over sodium sulfate
  7. 7
    Filtrationafter filtration
  8. 8
    Concentrationconcentrated under reduced pressure
  9. 9
    AutreThe residue was purified by a silica gel column

Mode opératoire

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).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US09072734B2uspto-grants-2015_07