Reaktion #65754

Reaktionsgleichung

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

phenylphosphonic dichloride

→

2-Chloro-3,4-diethoxycarbonyl-6-methyl-5-nitropyridine

Lösungsmittel

Water

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 over magnesium sulfate
4. 4
   workup.DISTILLATIONAfter the solvent was distilled off
5. 5
   Sonstigethe residue was purified by silica gel column chromatography (eluent:ethyl acetate)
6. 6
   Sonstigeto give an oily product

Vorschrift

To 1.0 g of 3,4-diethoxycarbonyl-6-methyl-5-nitro-2-pyridone was added 1.3 ml (3.2 eq.) of phenylphosphonic dichloride. The mixture was heated at 170° C. for 20 mintues. Water was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. After the solvent was distilled off, the residue was purified by silica gel column chromatography (eluent:ethyl acetate) to give an oily product.

Quelle