反应详情

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, was charged 1.2 L of Dowtherm A (a eutectic mixture of 26.5% diphenyl and 73.5% diphenyl oxide). The Dowtherm A was then preheated to 250° C. To this was cautiously added in small portions 48 g (0.11 moles) of 3-(4-acetylamino-phenylamino)-3-(4-cyclohexylphenyl)-acrylic acid butyl ester. As portions were added gas was evolved and foaming occurred. Crystals of product begin to form and adhere to the sides. After all the material had been added the heating of the reaction was continued for 1 hour. The mixture was then cooled to room temperature and hexane was added. The 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. customInto a 2 L three-neck round-bottom flask equipped with a condenser, magnetic stirrer
2. temperaturethermocouple, heating mantle with a variable voltage controller, and a nitrogen inlet
3. customwas then preheated to 250° C
4. additionAs portions were added gas
5. customto form
6. additionAfter all the material had been added the
7. temperatureheating of the reaction
8. filtrationThe 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