反应详情

A suspension of 2-cyano-N-(2,4-dichloro-5-methoxyphenyl)acetamide (3.2 g, 12.4 mmol) and [3-iodo-4-(2-methoxyethoxy)phenyl]amine (4.0 g, 13.7 mmol) in 350 mL of iso-propanol was heated to reflux and triethylorthoformate (5.6 mL, 33.7 mmol) was added dropwise. The reaction mixture was heated at reflux for 3 hours. Additional triethylorthoformate (2.0 mL, 12.0 mmol) was added dropwise and the reaction mixture was heated at reflux overnight. The mixture was allowed to cool to room temperature and the solid was collected by filtration, washed with iso-propanol, diethyl ether, and ethyl acetate and then dried in vacuo to give 5.5 g of 2-cyano-N-(2,4-dichloro-5-methoxyphenyl)-3-{[3-iodo-4-(2-methoxyethoxy)phenyl]amino}acrylamide as a yellow solid, mp 209-210° C.; MS (ES) 560.0, 562.1 (M−H)−

1. temperaturewas heated
2. temperatureto reflux
3. temperatureThe reaction mixture was heated
4. temperatureat reflux for 3 hours
5. temperaturethe reaction mixture was heated
6. temperatureat reflux overnight
7. filtrationthe solid was collected by filtration
8. washwashed with iso-propanol, diethyl ether, and ethyl acetate
9. customdried in vacuo