反应详情

温度

75 °C

To a suspension of ethyl 5-(4-(trifluoromethyl)phenyl)isoxazole-3-carboxylate (3.3 g, 11.6 mmol) in acetic acid (60 mL) was added N-chlorosuccinimide (3.1 g, 23.2 mmol). Upon heating to 75° C., a homogenous solution formed. After heating for 16 hours a further portion of N-chlorosuccinimide (1.5 g, 11.2 mmol) was added and the reaction was heated at 75° C. for another 16 hours. After cooling to ambient temperature, the reaction mixture was poured over ice. The white crystals which formed were collected by vacuum filtration and purified by silica gel chromatography, eluting with dichloromethane to obtain the title compound (3.2 g, 10.0 mmol).

1. customa homogenous solution formed
2. additionwas added
3. temperaturethe reaction was heated at 75° C. for another 16 hours
4. temperatureAfter cooling to ambient temperature
5. additionthe reaction mixture was poured over ice
6. customThe white crystals which formed
7. filtrationwere collected by vacuum filtration
8. custompurified by silica gel chromatography
9. washeluting with dichloromethane