Reaktion #75480

ord-f864972e90794ee39827fc1c7b384905

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    TemperaturThe reaction mixture was refluxed under N2 for 22 h
  3. 3
    SonstigeThe solvent was evaporated
  4. 4
    WaschenThe solid residue was washed with EtOH
  5. 5
    Sonstigewas dried under high vacuum

Vorschrift

To a mixture of 2,4-difluoroaniline (25 mmol, 3.2 g) in EtOH (10 mL) in an ice bath was added nitric acid (69% aq soln.; 1.8 mL) dropwise. After completion of the addition cyanamide (50% aq. soln.; 4 mL) was added. The reaction mixture was refluxed under N2 for 22 h. The solvent was evaporated. The solid residue was washed with EtOH and was dried under high vacuum to afford the title compound as a purple solid (2.32 g, 40%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06699854B2uspto-grants-2004_03