反应详情

温度

250 °C

In a 3 L three-neck flask, equipped with mechanical stirrer, Claisen adapter holding a thermocouple probe and reflux condenser with nitrogen inlet was added 0.75 L of Dowtherm A (a eutectic mixture of 26.5% diphenyl and 73.5% diphenyl oxide) The solvent is then preheated to 250° C. To this was cautiously added in small portions 77.0 grams (0.215 moles) of 3-(4-nitro-phenylamino)-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 grams (96.0%) of the title compound.

1. customIn a 3 L three-neck flask, equipped with mechanical stirrer
2. temperaturereflux condenser with nitrogen inlet
3. customis then preheated to 250° C
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