HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → 3-(3-Bromophenyl)isoxazol-5-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 3-(3-Bromophenyl)-3-oxopropanenitrile | HCID 2756839 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | 3-(3-Bromophenyl)isoxazol-5-amine | HCID 18526076 | — |
Reaction Steps
To a solution of 3-(3-bromophenyl)-3-oxopropanenitrile (1.12 g; 5.00 mmol; Note 1) in EtOH (20 mL) was added a solution of hydroxylamine hydrochloride (1.74 g; 25 mmol) and NaOAc (2.46 g; 30 mmol) in water (20 mL). The mixture was heated under reflux for 1 h, cooled and concentrated in vacuo. The residue was slurried in 1N NaOH and extracted with Et2O (×1). The organic layer was washed (water, brine), dried over Na2SO4 and concentrated in vacuo affording the title compound as a pale yellow solid which was used without further purification. LC/MS (method B) 2.21 min, m/z 239, 241 (Br isotopes).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08822518B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-c39b54f1fa1b4954b6e76d35b6f8f2a0 |
| Source note | uspto-grants-2014_09 |