Reaktion #159939

ord-5ec2d21edca24238b918011c1f187676

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturunder reflux for 24 hours
  3. 3
    workup.DISTILLATIONAfter distilling the solvent off, water
  4. 4
    workup.ADDITIONwas added to the residue
  5. 5
    Extraktionextracted with ethyl acetate
  6. 6
    WaschenThe organic layer was washed with brine
  7. 7
    Trocknendried over magnesium sulfate
  8. 8
    Sonstigeremoved of the solvent by distillation

Vorschrift

A mixture of ethyl 4-fluoro-3-nitrobenzoate 4.26 g, 2-isopropylimidazole 2.20 g, N,N-diisopropylethylamine 5.2 mL and acetonitrile 40 mL was heated under reflux for 24 hours. After distilling the solvent off, water was added to the residue and extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate and removed of the solvent by distillation, to provide 4.95 g of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829000B2uspto-grants-2014_09