反应详情

温度

250 °C

1.2 L of Dowtherm A was charged into a 2 L three neck round bottom flask equipped with a condenser, magnetic stirrer, thermocouple, heating mantle with a variable voltage controller, and a nitrogen inlet. The solvent was heated to 250° C. and 3-(4-acetylaminophenylamino)-3-(4-cyclohexylphenyl)-acrylic acid butyl ester 48 g (0.11 moles) was cautiously added in small portions. As portions were added gas was evolved and foaming occurred. Crystals of product began to form and adhere to the sides of the vessel. After all material had been added heating of the mixture was continued for 1 hour. The mixture was then cooled to room temperature and hexane added. A solid product was collected by vacuum filtration and washed with hexane. After drying in a vacuum oven, 35.7 g (90%) of product was recovered.

1. customequipped with a condenser, magnetic stirrer
2. temperaturethermocouple, heating mantle with a variable voltage controller, and a nitrogen inlet
3. additionAs portions were added gas
4. customto form
5. additionAfter all material had been added
6. temperatureheating of the mixture
7. temperatureThe mixture was then cooled to room temperature
8. filtrationA solid product was collected by vacuum filtration
9. washwashed with hexane
10. dry with materialAfter drying in a vacuum oven, 35.7 g (90%) of product
11. customwas recovered