Hydrogen Peroxide → HCID 20725604, compound

Temperature

80 °C

A mixture of 7.74 g of 3-methoxymethylpyridine, 60 ml of acetic acid and 7.5 g of 30% hydrogen peroxide solution was stirred while heating at 80° C. for four hours. The reaction mixture was cooled to room temperature, and then sodium carbonate was added in small portions. The reaction mixture was subjected to filtration, and washed with ethyl acetate. The resultant filtrate was washed with a saturated aqueous solution of sodium hydrogensulfite and a saturated sodium chloride solution, and dried over anhydrous sodium carbonate. Activated carbon was added, followed by filtration through Celite™. The filtrate was concentrated under reduced pressure to give 2.66 g of 3-methoxymethylpyridine N-oxide.

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationThe reaction mixture was subjected to filtration
3. washwashed with ethyl acetate
4. washThe resultant filtrate was washed with a saturated aqueous solution of sodium hydrogensulfite
5. dry with materiala saturated sodium chloride solution, and dried over anhydrous sodium carbonate
6. additionActivated carbon was added
7. filtrationfollowed by filtration through Celite™
8. concentrationThe filtrate was concentrated under reduced pressure

ORD record

ord-e58c21cc6e384f8a88263d6c280fd794

Source dataset

uspto-grants-2012_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08324387B2