Reaktion #159941

ord-9f5f1f17f6ec42e3a4aec68ef13ac7a5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturunder reflux for 15 hours in nitrogen atmosphere
  3. 3
    SonstigeFrom the reaction liquid the solvent
  4. 4
    workup.DISTILLATIONwas distilled off
  5. 5
    workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
  6. 6
    SonstigeThe organic layer was separated
  7. 7
    Waschenwashed with water
  8. 8
    Trocknendried over magnesium sulfate
  9. 9
    workup.DISTILLATIONDistilling the solvent off, 13.16 g of the title compound
  10. 10
    Sonstigewas obtained

Vorschrift

Ethyl 4-fluoro-3-nitrobenzoate 9.16 g, 2-(1-ethylpropyl)-1H-imidazole 5.94 g, N,N-diisopropylethylamine 11.2 mL and acetonitrile 86 mL were mixed and heated under reflux for 15 hours in nitrogen atmosphere. From the reaction liquid the solvent was distilled off, and the residue was dissolved in ethyl acetate and rendered weakly alkaline with saturated aqueous sodium hydrogencarbonate solution. The organic layer was separated, washed with water and dried over magnesium sulfate. Distilling the solvent off, 13.16 g of the title compound was obtained.

Quelle

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