preparation | in a three-mouth flask equipped with a mechanical stirring device and a reflux condenser tube, 80mL of methanol and 5-bromo -2-hydroxy isonicotinic acid are filled, 1.0mL of concentrated sulfuric acid is slowly added dropwise at room temperature, and the reflux reaction is carried out for 30h (thin layer chromatography tracking). At the end of the reaction, concentrate to 30mL, pour into 60mL of water, extract twice with 20mL of ether, wash the ether layer once with 5% sodium carbonate solution, then wash to neutral, dry with anhydrous magnesium sulfate, and evaporate to remove ether to obtain methyl 5-bromo-2-hydroxyisonicotinate. |