HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1-(2,6-Difluoropyridin-3-yl)ethanone oxime
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Hydroxylamine, sulfate (1:1) | HCID 159255 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 1-(2,6-Difluoropyridin-3-yl)ethanone | HCID 25132244 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 1-(2,6-Difluoropyridin-3-yl)ethanone oxime | HCID 86612608 | 53.3% |
Reaction Steps
Hydroxylamine sulfate (13.1 g) and sodium acetate (10.9 g) were added to a solution of 1-(2,6-difluoropyridin-3-yl)ethanone (4.18 g) in aqueous THF (50%, 200 mL), and the reaction solution was stirred at room temperature overnight. Water and ethyl acetate were added to the reaction solution, and the organic layer was separated. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (carrier: Chromatorex NH; elution solvent: ethyl acetate) to obtain 2.44 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07618960B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-a75dc279982e41d9862c702a9f9fe17a |
| Source note | uspto-grants-2009_11 |