Reaktion #1605812

ord-c1a270181535486187596470ab6be54a

Reaktionsgleichung

CC(=O)Nc1ccccc1-c1ccccc1
2-Phenyl-N-acetylaniline
Br
hydrogen bromide
CC(=O)Nc1ccc(Br)cc1-c1ccccc1
2-phenyl-4-bromo-N-acetylaniline
Ausbeute 91.3%

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe 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
    FiltrationThe precipitate was collected by filtration
  5. 5
    Waschenwashed with ethanol/water (=1:1)
  6. 6
    Sonstigedried under reduced pressure

Vorschrift

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).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09072734B2uspto-grants-2015_07