HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → 5-(5-Bromopyridin-3-yl)isoxazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | 1-(5-Bromopyridin-3-yl)-3-(dimethylamino)prop-2-ene-1-one | HCID 67057279 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 5-(5-Bromopyridin-3-yl)isoxazole | HCID 68027729 | — |
Reaction Steps
Hydroxyamine•hydrochloride (42 mg) was added to a methanol (2 ml) solution containing 1-(5-bromopyridin-3-yl)-3-(dimethylamino)prop-2-ene-1-one obtained in the 1st step, followed by reflux for 2 hours. The solvent was distilled away under reduced pressure, and water was added to the obtained residue, followed by extraction with ethyl acetate. Then, the organic layer was washed with saturated saline and dried over anhydrous sodium sulfate, and the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:0 to 1:3), and a white solid of 5-(5-bromopyridin-3-yl)isoxazole (59.5 mg) was thus obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772320B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-a4bb2d2ab04045f3887803fb1c7964c6 |
| Source note | uspto-grants-2014_07 |