Reaktion #45930

ord-da35513542f84da8825139e72ef6d024

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction was quenched by cold H2O (50 mL)
  2. 2
    Extraktionthe resulting mixture was extracted with EtOAc (3×100 mL)
  3. 3
    WaschenThe combined EtOAc extracts were washed with brine (3×50 mL)
  4. 4
    Trocknendried (anhydrous Na2SO4)
  5. 5
    SonstigeThe solvent was removed in vacuo

Vorschrift

To a stirred solution of 6-(3-diethylaminopropoxy)-2,4-difluoronitrobenzene (11 mmol) and triethylamine (22 mmol) in DMF (20 mL), a solution of n-butylamine (11 mmol) in DMF (8 mL) was added dropwise at rt, and the mixture was stirred at rt for 10 h. The reaction was quenched by cold H2O (50 mL), and the resulting mixture was extracted with EtOAc (3×100 mL). The combined EtOAc extracts were washed with brine (3×50 mL) and dried (anhydrous Na2SO4). The solvent was removed in vacuo to afford the desired 2-n-butylamino-6-(3-diethylaminopropoxy)-4-fluoronitrobenzene which was used for further transformation.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737285B2uspto-grants-2010_06