反应详情

To a suspension of 2-cyano-N-(2,4-dichloro-5-methoxyphenyl)acetamide (5.44 g, 21.0 mmol) in 350 mL of iso-propanol, under N2, was added (4-ethoxy-3-iodophenyl)amine (5.0 g, 19.30 mmol). This mixture was heated to reflux and triethylorthoformate (8.53 mL, 51.30 mmol) was added dropwise and the reaction mixture was heated at reflux overnight. The mixture was allowed to cool to room temperature and the yellow solid was collected by filtration, washed with iso-propanol, and dried overnight at ˜40° C. under reduced pressure to give 5.46 g (54%) of 2-cyano-N-(2,4-dichloro-5-methoxyphenyl)-3-[(4-ethoxy-3-iodophenyl)amino]prop-2-enamide as a yellow solid, mp >245° C.; MS (EI) m/z 531.01 (M)+

1. temperatureThis mixture was heated
2. temperatureto reflux
3. temperaturethe reaction mixture was heated
4. temperatureat reflux overnight
5. filtrationthe yellow solid was collected by filtration
6. washwashed with iso-propanol
7. customdried overnight at ˜40° C. under reduced pressure