Réaction #77252

ord-0a960065e0924f689f305d413ebcea84

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Extractionextracted three times with ethyl acetate
  2. 2
    FiltrationThe combined organic layers are filtered through Celite
  3. 3
    Séchagedried over anhydrous magnesium sulfate
  4. 4
    Concentrationconcentrated in vacuo

Mode opératoire

To a mixture of 2-(4-fluoro-5-nitrobenzoyl)-3-methylpyridine (7.13 g, 0.0258 mol) and glacial acetic acid at 70-80° C. is added iron powder (7.76 g, 0.130 mol) in three portions. The resultant mixture is stirred overnight at 70-80° C., cooled to room temperature and extracted three times with ethyl acetate. The combined organic layers are filtered through Celite, dried over anhydrous magnesium sulfate and concentrated in vacuo to afford the title compound as a tan solid (4.36 g, 69.8%) which is identified by NMR spectral analysis.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06706663B2uspto-grants-2004_03