3-bromo-2-methylpyridine 1-oxide synthesis

Yield:97944-32-6 94.25%

Reaction Conditions:

with 3-chloro-benzenecarboperoxoic acid in dichloromethane at 30; for 8 h;Cooling with ice;

Steps:

step one:

3-Bromo-2-methylpyridine (compound 1, 96.0 g, 558.1 mmol) was weighed and dissolved in 600 mL of dichloromethane.Under an ice bath, m-chloroperoxybenzoic acid (m-CPBA, 135.9 g, 669.6 mmol) was added in portions, and the temperature was raised to 30° C. and stirring was continued for 8 hours.A small sample was quenched with 15% sodium sulfite solution, and LC-MS monitoring showed that compound 1 was consumed;The reaction was stopped, the reaction solution was completely quenched and then liquid-separated, and the organic phase was concentrated to obtain 98.9 g of light yellow solid3-Bromo-2-methylpyridine-N-oxide (compound 2, yield 94.25%).

References:

CN114380738,2022,A Location in patent:Paragraph 0014-0015