Reaktion #10870

Reaktionsgleichung

3,4-difluoronitrobenzene

N-methylpiperazine

→

1-(2-fluoro-4-nitrophenyl)-4-methylpiperazine

Ausbeute 97.0%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 3 h
2. 2
   Sonstigethe solvent was evaporated under reduced pressure
3. 3
   Sonstigethe residue was partitioned between water and ethyl acetate (200 mL each)
4. 4
   ExtraktionThe aqueous layer was extracted with ethyl acetate (3×200 mL)
5. 5
   Waschenthe combined organic layers were then washed with water and brine (200 mL each)
6. 6
   Trocknendried (MgSO4)
7. 7
   Filtrationfiltered
8. 8
   Sonstigeevaporated under reduced pressure

Vorschrift

A solution of 3,4-difluoronitrobenzene (12.00 g, 75.4 mmol) (Aldrich) and N-methylpiperazine (18.89 g, 188.6 mmol) in acetonitrile (150 mL) was heated at reflux for 3 h. The reaction mixture was allowed to stand overnight at room temperature, then the solvent was evaporated under reduced pressure and the residue was partitioned between water and ethyl acetate (200 mL each). The aqueous layer was extracted with ethyl acetate (3×200 mL) and the combined organic layers were then washed with water and brine (200 mL each), dried (MgSO4), filtered, and evaporated under reduced pressure to give 1-(2-fluoro-4-nitrophenyl)-4-methylpiperazine as a pale brown solid (17.5 g, 97%, mp 68–70° C.).

Quelle