HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → 2,6-Dichloropyridine N-Oxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 2,6-Dichloropyridine | HCID 16989 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2,6-Dichloropyridine N-Oxide | HCID 817673 | — |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05656648 |
| Source dataset | uspto-grants-1997_08 |
| ORD ID | ord-b7277cc43feb4ab4bb35483a545b7bd3 |
| Source note | uspto-grants-1997_08 |