Réaction #61171

ord-73ecc3b717224c47a915a4cc25aca307

Réactifs

Aucun

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Concentrationconcentrated in vacuo
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in EtOAc (100 mL)
  3. 3
    Lavagewashed with water (2×100 mL)
  4. 4
    Séchagedried (Na2SO4)
  5. 5
    Concentrationconcentrated in vacuo
  6. 6
    AutrePurification by silica gel column chromatography

Mode opératoire

To a solution of 2,4-difluoronitrobenzene (2.09 g, 13.1 mmol) in EtOH (10 mL) at ambient temperature was added piperidine (3.35 g, 39.4 mmol) dropwise. The reaction was allowed to stir overnight and concentrated in vacuo. The residue was dissolved in EtOAc (100 mL), washed with water (2×100 mL), dried (Na2SO4) and concentrated in vacuo. Purification by silica gel column chromatography afforded 1.10 (37%) of the title compound as an oil. Mass spectrum (ESI, m/z): Calcd. for C11H13FN2O2, 225.1 (M+H), found 225.1.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07427683B2uspto-grants-2008_09