反应详情

温度

62 °C

Sodium hydride (2.87 g, 60%, 71.8 mmol) was added slowly to methanol (62.5 mL) with stirring. 6-Hydroxy-nicotinic acid (5 g, 35.9 mmol) was added slowly, and the reaction mixture was heated to 62° C. Iodomethane (8.96 mL, 143.7 mmol) was added and the reaction was stirred overnight. The mixture was then cooled to room temperature and filtered to remove undissolved starting material. The filtrate was concentrated to yield a yellow powder which NMR analysis showed contained the title compound and methyl 1-methyl-6-oxo-1,6-dihydropyridine-3-carboxylate. This mixture was used in the subsequent reaction.

1. stirringthe reaction was stirred overnight
2. temperatureThe mixture was then cooled to room temperature
3. filtrationfiltered
4. customto remove undissolved
5. concentrationThe filtrate was concentrated
6. customto yield a yellow powder which NMR analysis