HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxylamine → HCID 178510829, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxylamine | HCID 787 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 68527071 | HCID 68527071 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178510829 | HCID 178510829 | — |
Reaction Steps
To a solution of 3,4-dichloro-N-[6-(4-cyanomethylphenoxy)pyridin-3-yl]benzamide (700 mg, 1.76 mmol) in ethanol (30 mL) were added water (2 mL), hydroxylamine (420 mg, 12.71 mmol) and potassium carbonate (1.76 g, 12.73 mmol). Under argon, the resulting solution was stirred under reflux for 4 hours. The resulting reaction solution was concentrated under reduced pressure. To the residue was added water, and extracted with ethyl acetate. The ethyl acetate layer was washed with brine, dried over anhydrous magnesium sulfate, evaporated, and the residue was purified by silica gel column chromatography (dichloromethane:methanol=10:1), to thereby yield 510 mg of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08236826B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-4bf3391dfcf046f280897359aa365134 |
| Source note | uspto-grants-2012_08 |