反应详情

温度

250 °C

Dowtherm A, 0.75 L, was placed in a 3 L three-neck flask, equipped with mechanical stirrer, Claisen adapter holding a thermocouple probe and reflux condenser with nitrogen inlet and heated to 250° C. To this was cautiously added in small portions 77.0 grams (0.215 moles) of 3-(4-nitrophenylamino)-3-(3-fluorophenyl) acrylic acid butyl ester over the course of 0.25 hours. The mixture was maintained at 250° C. for 1.5 hours and then allowed to cool to 90° C. over the course of 2 hours. The mixture was treated with 1.0 L of hexanes, and allowed to cool to room temperature while stirring overnight. The tan solids were collected by suction filtration and washed with three 0.15 L portions of hexanes. The solids were dried under vacuum at 50° C. overnight to yield 58.63 g (96.0%) of the title compound.

1. customequipped with mechanical stirrer
2. temperaturereflux condenser with nitrogen inlet
3. temperatureThe mixture was maintained at 250° C. for 1.5 hours
4. temperatureto cool to 90° C. over the course of 2 hours
5. temperatureto cool to room temperature
6. filtrationThe tan solids were collected by suction filtration
7. washwashed with three 0.15 L portions of hexanes
8. customThe solids were dried under vacuum at 50° C. overnight