反应详情

温度

45 °C

A suspension of 5,6-dichloropyridine-2-carboxylic acid-N-oxide (5.0 g, 24.0 mmol) in methanol (100 mL) was saturated with HCl gas and the reaction mixture heated at 40-50° C. for one hour. The solvent was removed and the residue dissolved in diethyl ether/ethyl acetate. The organic solution was washed with water, saturated sodium bicarbonate solution, brine, dried, and concentrated to give methyl 5,6-dichloropyridine-2-carboxylate-N-oxide (4.0 g, 18.1 mmol). 1H NMR (DMSO-d6): δ 7.75 (s, 2H), 3.88 (s, 3H).

1. customThe solvent was removed
2. dissolutionthe residue dissolved in diethyl ether/ethyl acetate
3. washThe organic solution was washed with water, saturated sodium bicarbonate solution, brine
4. customdried
5. concentrationconcentrated