Reaktion #49283

ord-95cd312236934178bc6fff74326d23f0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with ethyl acetate
  2. 2
    WaschenThe organic layer was washed with saturated brine
  3. 3
    Trocknendried over anhydrous sodium sulfate
  4. 4
    SonstigeThe solvent was evaporated under reduced pressure
  5. 5
    Sonstigethe residue was purified by slurry

Vorschrift

3-Chlorobenzoylchloride (110.0 g, 57.1 mmol) was dissolved in dichloromethane (200 mL), and the solution was added with cumylamine (9.04 mL, 62.9 mmol), triethylamine (12.0 mL, 85.7 mmol) and DMAP (698 mg, 5.71 mmol), followed by stirring at room temperature for 3 hours. The reaction mixture was added with water, extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by slurry using diisopropyl ether to obtain 3-chloro-N-(1-methyl-1-phenylethyl)benzamide (15.0 g, yield 96%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745641B2uspto-grants-2010_06