HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → (3-Chloro-4-isoxazol-5-yl-phenyl)-carbamic Acid Tert-butyl Ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 54077142 | HCID 54077142 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | (3-Chloro-4-isoxazol-5-yl-phenyl)-carbamic Acid Tert-butyl Ester | HCID 54457472 | — |
Reaction Steps
A solution of [3-chloro-4-(3-dimethylamino-acryloyl)-phenyl]-carbamic acid tert-butyl ester (270 mg) in dioxane (3 ml) is treated with hydroxylamine hydrochloride (122 mg) and the mixture is stirred at room temperature for 10 days. The mixture is diluted with ethyl acetate, washed successively with water, 5% aqueous sodium bicarbonate, saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. The solvent is removed by evaporation under reduced pressure and the resulting residue is chromatographed over silica gel (33% ethyl acetate in hexanes is used as the eluant) to provide the desired product as a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06380243B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-63d7cbf842774cdca8329945b34b0cec |
| Source note | uspto-grants-2002_04 |