1112213-20-3

175358-01-7

1112213-20-3

Step 3: Preparation of methyl 3-amino-6-chloropyridine-2-carboxylate hydrochloride; 3-amino-6-chloropyridine-2-carboxamide (0.87 g, 5.09 mmol) was mixed with 35% hydrochloric acid (5 mL) and the reaction was heated at 110°C for 5 hours. After completion of the reaction, the solvent was removed by distillation under reduced pressure to give 3-amino-6-chloropyridine-2-carboxylic acid hydrochloride (1.22 g, 98% yield). Mass spectrum (electrospray positive ion mode): m/z 246 [M+H]+. Subsequently, 3-amino-6-chloropyridine-2-carboxylic acid hydrochloride (1.2 g, 4.89 mmol) was suspended in methanol (10 mL), thionyl chloride (0.85 mL, 6.36 mmol) was added slowly and dropwise at room temperature, and the reaction mixture was stirred for 24 hr. at 100 °C. At the end of the reaction, the solvent was removed by distillation under reduced pressure to afford methyl 3-amino-6-chloropyridine-2-carboxylate hydrochloride (1.21 g, 95% yield). Mass spectrum (electrospray positive ion mode): m/z 260 [M+H]+.