反应详情

15 ml of thionyl chloride were added to a solution of 5.22 g (0.0216 moles) of 3-difluoromethoxy-2,4,5-trifluorobenzoic acid [(XII), R1 --OCHF2, R3' =H, X=X'=F] (prepared as described in Preparation 1, 2 or 3) in 300 ml of benzene, and the mixture was heated under reflux for 3 hours. At the end of this time, benzene and excess thionyl chloride were removed by distillation under reduced pressure, to give 3-difluoromethoxy-2,4,5-trifluorobenzoyl chloride [(XIII), R1 =--OCHF2, R3' =H, X=X'=F].

1. temperaturethe mixture was heated
2. temperatureunder reflux for 3 hours
3. customAt the end of this time, benzene and excess thionyl chloride were removed by distillation under reduced pressure