Water → Pyridine, 2,3-dimethyl-, 1-oxide

Temperature

95 °C

71.79 g of 2,3-dimethylpyridine (II) was dissolved in 240 ml of acetic acid, to which 40 ml of 30% hydrogen peroxide solution was added and the resulting mixture was heated at 95° C. for 3 hours. Furthermore, 18 ml of a 30% hydrogen peroxide solution was added to the mixture and heated at 95° C. for 13 hours, and thereafter, 700 ml of water was added thereto and the resulting mixture was neutralized with sodium carbonate and extracted with chloroform. The resulting organic layer was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The resulting precipitation was recrystallized from diisopropylether to obtain 71.34 g of 2,3-dimethylpyridine N-oxide (III).

1. additionwas added
2. temperatureheated at 95° C. for 13 hours
3. extractionextracted with chloroform
4. dry with materialThe resulting organic layer was dried over anhydrous sodium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customThe resulting precipitation
7. customwas recrystallized from diisopropylether

ORD record

ord-5db019416a4342aa958ad1ddfeb901d1

Source dataset

uspto-grants-2003_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06525066B2