Reaktion #65746

Reaktionsgleichung

3,4-diethoxycarbonyl-5-nitro-6-phenyl-2-pyridone

phenylphosphonic dichloride

→

2-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine

Lösungsmittel

Water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe mixture was extracted with ethyl acetate
2. 2
   WaschenThe organic layer was washed with water
3. 3
   Trocknena saturated aqueous solution of sodium chloride, and dried over magnesium sulfate
4. 4
   workup.DISTILLATIONThe solvent was distilled off
5. 5
   Sonstigethe residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane 1:2)
6. 6
   Sonstigeto give an oily product

Vorschrift

To 1.0 g of 3,4-diethoxycarbonyl-5-nitro-6-phenyl-2-pyridone was added 1.3 ml (3.37 eq.) of phenylphosphonic dichloride, and the mixture was heated at 150° C. for 2.5 hours. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate. The solvent was distilled off, and the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane 1:2), to give an oily product. Yield: 950 mg (90.5%).

Quelle