Hydrogen peroxide water → Pyridine, 4-chloro-3-methoxy-2-methyl-, 1-oxide

Temperature

90 °C

36.98 g of 4-chloro-3-methoxy-2-methylpyridine (V) was dissolved in 685 ml of acetic acid and 92 ml of hydrogen peroxide water was added thereto and the resulting mixture was heated at 90° C. for 24 hours, and thereafter, the reaction solution was distilled off under reduced pressure. The resulting residue was dissolved in chloroform and washed with saturated sodium bicarbonate solution, and saturated salt water, and thereafter, dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 37.64 g of 4-chloro-3-methoxy-2-methylpyridine N-oxide (VI).

1. distillationthe reaction solution was distilled off under reduced pressure
2. dissolutionThe resulting residue was dissolved in chloroform
3. washwashed with saturated sodium bicarbonate solution, and saturated salt water
4. dry with materialdried over anhydrous sodium sulfate
5. distillationThe solvent was distilled off under reduced pressure

ORD record

ord-33f6df645d154677aa5c5b80a33a661c

Source dataset

uspto-grants-2003_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06525066B2