Reaktion #65762

Reaktionsgleichung

hydrochloric acid

2-chloro-3,4-diethyoxycarbonyl-6-(4-methoxyphenyl)-5nitropyridine

→

3-Amino-6-chloro-4,5-diethoxycarbonyl-2-(4-methoxyphenyl)pyridine

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   Temperaturthe mixture was refluxed
3. 3
   TemperaturAfter heating for 20 minutes
4. 4
   workup.DISTILLATIONthe solvent was distilled off
5. 5
   Extraktionfollowed by extraction with ethyl acetate
6. 6
   FiltrationAfter the precipitate was filtered off
7. 7
   Waschenthe obtained organic layer was washed with water
8. 8
   Trocknena saturated aqueous solution of sodium chloride, and dried
9. 9
   workup.DISTILLATIONThereafter, the solvent was distilled off

Vorschrift

In 4 ml of ethanol was dissolved 280 mg of 2-chloro-3,4-diethyoxycarbonyl-6-(4-methoxyphenyl)-5nitropyridine, whereto 340 mg(8.9 eq.) of reduced iron was added. After the mixture was heated to 60° C., 1.5 ml of conc. hydrochloric acid was added dropwise and the mixture was refluxed. After heating for 20 minutes, the solvent was distilled off. The residue was neutralized with an aqueous solution of sodium hydrogencarbonate, followed by extraction with ethyl acetate. After the precipitate was filtered off, the obtained organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried. Thereafter, the solvent was distilled off.

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