Reaktion #65778

Reaktionsgleichung

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

1H-1,2,4-triazole

pyridine

→

title compound

3,4-Diethoxycarbonyl-5-nitro-6-phenyl-2-(1,2,4-triazol-1-yl)pyridine

Lösungsmittel

1,2-dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas reacted at 80° C. for 18 hours
2. 2
   EinengenAfter the reaction mixture was concentrated
3. 3
   Extraktionthe concentrate was extracted with ethyl acetate
4. 4
   WaschenThe extract was washed with water
5. 5
   Trocknena saturated aqueous solution of sodium chloride and dried over sodium sulfate
6. 6
   workup.DISTILLATIONAfter the solvent was distilled off

Vorschrift

A mixture of 0.379 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine, 0.2 g of (1H-1,2,4-triazole, 0.2 ml of pyridine and 15 ml of 1,2-dichloroethane was reacted at 80° C. for 18 hours. After the reaction mixture was concentrated, the concentrate was extracted with ethyl acetate. The extract was washed with water and a saturated aqueous solution of sodium chloride and dried over sodium sulfate. After the solvent was distilled off, the residue was subjected to silica gel column chromatography (eluent:dichloromethane/ethyl acetate 4:1), to give 0.19 g of the title compound as yellow crystals.

Quelle