Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 5006-66-6, name is 6-Oxo-1,6-dihydropyridine-3-carboxylic acid. A new synthetic method of this compound is introduced below., Formula: C6H5NO3
To a stirred solution of 6-hydroxynicotinic acid (10 g, 72 mmol) in absolute ethanol (500 mL) was added sulfuric acid (4 mL) at room temperature. The mixture was heated to reflux for 48 h. After cooling down to room temperature, water (50 mL) was added and the reaction mixture was neutralised to pH= 6-7 by portionwise addition of sodiumhydrogen carbonate (caution: gas evolution). The mixture was evaporated under reduced pressure (most of ethanol was removed), and the residue was extracted with ethyl acetate (3 × 50 mL). The combined organic extracts were washed with brine, dried over Na2SO4 and evaporated under reduced pressure leading to the pure ethyl 6-hydroxynicotinate[30] (10 g, 86percent). 1H NMR (400 MHz, CDCl3): delta 13.07 (s,1H), 8.14 (s, 1H), 7.94 (d, 1H, J = 9.9 Hz), 6.51 (d, 1H, J = 9.4 Hz),4.25 (q, 2H, J =7.1 Hz), 1.29 ppm.To a stirred solution of lithium aluminium hydride (1.4 g, 37 mmol,1.2 equiv.) in anhydrous THF (20 mL) at room temperature was added dropwise over 1 h a solution of ethyl 6-hydroxynicotinate (5.1 g,31 mmol) in anhydrous THF (150 mL) at the same temperature. The mixture was stirred at room temperature for 2 h and then heated toreflux for 30 min. The reaction mixture was cooled down to 0 °C andquenched with ethyl acetate (12 mL) and water (6 mL). The solventswere removed and the residue was taken up in refluxing ethanol(200 mL). The solution was filtered through Celite® and ethanol was evaporated under reduced pressure. The crude material was purified bycolumn chromatography on silica gel with ethyl acetate/methanol(75:25) as eluent to afford the pure title compound 12 (2.3 g, 60percent).
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Reference:
Article; Landelle, Gregory; Schmitt, Etienne; Panossian, Armen; Vors, Jean-Pierre; Pazenok, Sergiy; Jeschke, Peter; Gutbrod, Oliver; Leroux, Frederic R.; Journal of Fluorine Chemistry; vol. 203; (2017); p. 155 – 165;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem