反应详情

Hydroxylamine hydrochloride (6.14 g, 88.0 mmol) was added to a suspension of ethyl 4-(4-tert-butylphenyl)-2,4-dioxobutanoate (20.4 g, 73.7 mmol) in absolute ethanol (300 mL) and the reaction was heated to reflux for 3 hours. After cooling to room temperature, the organics were removed in vacuo and the resulting residue was purified by silica gel chromatography, eluting with heptane to 10% methanol in dichloromethane, to obtain afford the title compound white solid was filtered, washed with water and cold ethanol and dried in vacuo to obtain ethyl 5-(4-tert-butylphenyl)isoxazole-3-carboxylate (15.9 g, 58.0 mmol).

1. temperaturethe reaction was heated
2. temperatureto reflux for 3 hours
3. customthe organics were removed in vacuo
4. customthe resulting residue was purified by silica gel chromatography
5. washeluting with heptane to 10% methanol in dichloromethane
6. customto obtain