Reaktion #61171

ord-73ecc3b717224c47a915a4cc25aca307

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated in vacuo
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in EtOAc (100 mL)
  3. 3
    Waschenwashed with water (2×100 mL)
  4. 4
    Trocknendried (Na2SO4)
  5. 5
    Einengenconcentrated in vacuo
  6. 6
    SonstigePurification by silica gel column chromatography

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07427683B2uspto-grants-2008_09