反应详情

温度

60 °C

38.5 g 4-chloro-2,5-difluorobenzoic acid (0.2 mole) was placed in a 250 mL, 3-necked roundbottom flask equipped with a magnetic stirbar, a thermometer, and a water-cooled condenser. 238 g thionyl chloride was added in one lot. The mixture was stirred and heated on a water bath. At about 58°-60° C. the solid dissolved with evolution of gas and formation of foam. The mixture was stirred and maintained at 60° C. until all the solid dissolved - about 30 minutes. It was then heated in a boiling water bath to reflux and held there for 2 hours.

1. customequipped with a magnetic stirbar
2. temperatureheated on a water bath
3. dissolutionAt about 58°-60° C. the solid dissolved with evolution of gas and formation of foam
4. stirringThe mixture was stirred
5. dissolutiondissolved - about 30 minutes
6. temperatureIt was then heated in a boiling water bath
7. temperatureto reflux