반응 #77252

ord-0a960065e0924f689f305d413ebcea84

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted three times with ethyl acetate
  2. 2
    여과The combined organic layers are filtered through Celite
  3. 3
    건조dried over anhydrous magnesium sulfate
  4. 4
    농축concentrated in vacuo

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06706663B2uspto-grants-2004_03