Reaktion #43586

ord-ae2de73b0a5c4c679f9b21e0b468d267

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewas removed under reduced pressure
  2. 2
    workup.ADDITIONThe reaction mixture was then treated with dichloromethane and water
  3. 3
    ExtraktionThe aqueous phase was extracted twice with dichloromethane
  4. 4
    Sonstigethe combined organic phases were dried
  5. 5
    Sonstigethe solvent was removed under reduced pressure

Vorschrift

To a solution of 3-fluoro-4,5-dihydroxybenzaldehyde (0.66 g, 4.2 mmol) in DMF (30 ml) was added potassium carbonate (1.15 g, 8.3 mmol) and 1,2-dibromoethane (0.72 ml, 8.3 mmol) and the resultant mixture was heated to 80° C. for 18 h before the solvent was removed under reduced pressure. The reaction mixture was then treated with dichloromethane and water. The aqueous phase was extracted twice with dichloromethane and the combined organic phases were dried and the solvent was removed under reduced pressure to give the desired compound as a cream solid (0.73 g, 95%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732461B2uspto-grants-2010_06