Reaktion #53546

ord-9446fc975140435fb7311e73e5cbd347

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux for 6 hrs
  2. 2
    Temperaturcooled
  3. 3
    Sonstigethe solvent removed under vacuum
  4. 4
    Extraktionthe product extracted with ethyl acetate (2×100 ml)
  5. 5
    TrocknenThe combined extracts were dried (Na2SO4)
  6. 6
    Sonstigeevaporated
  7. 7
    Sonstigethe residue recrystallised from ethanol
  8. 8
    Sonstigeto give a white solid

Vorschrift

5-Fluoro-2-(4′-amino-3′-iodophenyl)benzothiazole (5 g, 0.0135 mol), copper cyanide (3.65 g, 0.04 mol) and DMF (100 ml) were heated under reflux for 6 hrs, cooled and the solvent removed under vacuum. The residue was stirred in water (50 ml) for 30 mins, then the product extracted with ethyl acetate (2×100 ml). The combined extracts were dried (Na2SO4), evaporated and the residue recrystallised from ethanol to give a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06858633B1uspto-grants-2005_02