Reaktion #88236

Reaktionsgleichung

potassium carbonate

4-methyl-3-nitropyridin-2(1H)-one

phosphorus oxybromide

→

title compound

Ausbeute 71.8%

2-bromo-4-methyl-3-nitropyridine

Ausbeute 71.8%

Lösungsmittel

dichloroethane

dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeat the ambient temperature
2. 2
   TemperaturThe reaction mixture was refluxed for 12 hours
3. 3
   SonstigeThe organic layer was separated
4. 4
   Waschenwashed with water and brine
5. 5
   Trocknendried over sodium sulfate
6. 6
   SonstigeThe solvent was evaporated

Vorschrift

The 4-methyl-3-nitropyridin-2(1H)-one (110 g, 0.71 mol) was suspended in dichloroethane (1 L). The solution of phosphorus oxybromide (317 g, 1.1 mol) in dichloroethane (1 L) was added dropwise thereto at the ambient temperature. The reaction mixture was refluxed for 12 hours. The mixture was allowed to cool to room temperature, poured into ice water, and neutralized with potassium carbonate. The organic layer was separated, washed with water and brine, and dried over sodium sulfate. The solvent was evaporated to provide the title compound (yield 71.8%).

Quelle