Reaktion #77252

Reaktionsgleichung

2-(4-fluoro-5-nitrobenzoyl)-3-methylpyridine

→

title compound

Ausbeute 73.4%

3-Amino-4-fluorophenyl 3-methyl-2-pyridyl ketone

Ausbeute 73.4%

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle