反应详情

温度

5 °C

50% Sodium hydride (2.4 g, 0.05 mol) was washed with petroleum ether, suspended in dry toluene (50 ml) and stirred at 5° C. Ethyl 3-(2-methoxyphenylamino)acrylate (8.7 g, 0.05 mol) in dry toluene (25 ml) was added and the mixture was stirred for 2.5 hours. Benzoyl chloride (6.8 g, 0.05 mol) in dry toluene (25 ml) was added dropwise and the mixture was heated under reflux for 2 hours. The mixture was cooled, washed with dilute hydrochloric acid, water and brine, then dried and evaporated. The residue was chromatographed (silica gel, dichloromethane) to afford ethyl 2-benzoyl-3-(2-methoxyphenylamino)acrylate (7.62 g, 46.8%) as a yellow oil.

1. stirringthe mixture was stirred for 2.5 hours
2. temperaturethe mixture was heated
3. temperatureunder reflux for 2 hours
4. temperatureThe mixture was cooled
5. washwashed with dilute hydrochloric acid, water and brine
6. customdried
7. customevaporated
8. customThe residue was chromatographed (silica gel, dichloromethane)