Hydrogen Peroxide → 2,6-Dichloropyridine N-Oxide

24 g of 2,6-dichloropyridine, 200 ml of trifluoroacetic acid and 28 ml of 33% hydrogen peroxide are heated to 100° C. for 4 hours. The mixture is cooled, 600 ml of water are then added and the resulting mixture is concentrated under vacuum to a volume of 50-100 ml. It is alkalinized with sodium hydrogen carbonate and then extracted with DCM, and the organic phase is separated after settling has taken place and dried over sodium sulphate. It is filtered and concentrated under vacuum, and the residue is recrystallized from AcOEt to obtain 18.8 g of 2,6-dichloropyridine N-oxide; m.p.=138°-140° C.

1. temperatureThe mixture is cooled
2. concentrationthe resulting mixture is concentrated under vacuum to a volume of 50-100 ml
3. extractionextracted with DCM
4. customthe organic phase is separated
5. dry with materialdried over sodium sulphate
6. filtrationIt is filtered
7. concentrationconcentrated under vacuum
8. customthe residue is recrystallized from AcOEt

ORD record

ord-b7277cc43feb4ab4bb35483a545b7bd3

Source dataset

uspto-grants-1997_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05656648