Reaktion #65761

Reaktionsgleichung

sodium hydrogencarbonate

3,4-diethoxycarbonyl-6-(4-methoxyphenyl)-5-nitro-2(1H)pyridone

phosphorus oxychloride

→

2-Chloro-3,4-diethoxycarbonyl-6-(4-methoxyphenyl)-5-nitropyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionfollowed by extraction with ethyl acetate
2. 2
   WaschenThe organic layer was washed with water
3. 3
   Trocknena saturated aqueous solution of sodium chloride and dried
4. 4
   workup.DISTILLATIONThe solvent was distilled off
5. 5
   SonstigeThe residue was purified by silica gel column chromatography (eluent:ethyl acetate/hexane 1:1)

Vorschrift

To 300 mg of 3,4-diethoxycarbonyl-6-(4-methoxyphenyl)-5-nitro-2(1H)pyridone were added 0.5 ml of phosphorus oxychloride and two drops of DMF. The mixture was heated at 100° C. for 1 hour. After ice water was added, the mixture was neutralized with sodium hydrogencarbonate, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried. The solvent was distilled off. The residue was purified by silica gel column chromatography (eluent:ethyl acetate/hexane 1:1).

Quelle