반응 #40534

반응 방정식

4-hydroxy-6-methyl-2-pyrone

2-(aminomethyl)pyridine

→

title compound

수율 92.0%

4-Hydroxy-6-methyl-1-pyridin-2-ylmethyl-1H-pyridin-2-one

수율 92.0%

용매

water

반응 조건

후처리

1. 1
   온도the mixture heated
2. 2
   온도to reflux for 2.5 hours
3. 3
   여과The resulting light yellow compound was filtered from the cooled mixture

실험 절차

To a suspension of 12.6 g (0.1 mol) of 4-hydroxy-6-methyl-2-pyrone in 50 ml water was added 2-(aminomethyl)pyridine (10.3 ml, 0.1 mol) and the mixture heated to reflux for 2.5 hours. The resulting light yellow compound was filtered from the cooled mixture. Concentration of the filtrate and trituration of the resulting gum with dichloromethane afforded a second crop of the title compound (19.85 g, 92%). NMR (DMSO-d6, ppm): 10.5 (s, 1H), 8.5 (d, 1H), 7.7-7.8 (t, 1H), 7.2 (t, 1H), 7.1 (d, 1H), 5.8 (s, 1H), 5.5 (s, 1H), 5.2 (s, 2H), 2.2 (s, 3H). FIA: m/z-215.1 ES−/217.1 ES+

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