반응 #65759

반응 방정식

sodium nitrite

2-amino-3,4-diethoxycarbonyl-6-(4-methoxyphenyl)pyridine

hydrochloric acid

dioxane

→

3,4-Diethoxycarbonyl-6-(4-methoxyphenyl)-2-pyridone

용매

water

반응 조건

후처리

1. 1
   온도cooling
2. 2
   workup.DISTILLATIONThe solvent was distilled off
3. 3
   추출followed by extraction with ethyl acetate
4. 4
   세척The organic layer was washed with a saturated aqueous solution of sodium chloride
5. 5
   기타dried
6. 6
   workup.DISTILLATIONThe solvent was distilled off
7. 7
   기타The resulting crude crystals were recrystallized from ethanol

실험 절차

To 100 mg of 2-amino-3,4-diethoxycarbonyl-6-(4-methoxyphenyl)pyridine were added 2 ml of 1N hydrochloric acid and 5 ml of dioxane, and thereto was added dropwise a solution of 26 mg (1.3 eq.) of sodium nitrite dissolved in 0.5 ml of water under ice-cooling. The mixture was stirred at room temperature overnight. The solvent was distilled off. The residue was neutralized with sodium hydrogencarbonate, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried. The solvent was distilled off. The resulting crude crystals were recrystallized from ethanol.

출처