Xiong Guo-lan
2008
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Journal
Journal of Anhui Agricultural Sciences
Abstract
[Objective] The aim was to optimize the best technology of synthesis of 2,6-difluoroaniline with 2,6-Dichloro-cyanobenzene method.[Method] The 2,6-difluoroaniline was synthesized by using 2,6-Dichloro-cyanobenzene,the effect of each process parameter on the yields for reaction of fluoridation,hydrolysis,and Hofmann rearrangement was studied through single factor test.[Result] The optimal process conditions of fluoridation reaction were: DCBN/KF was 1.0∶2.8,temperature 170-180 ℃ in the early stage for 2 h,temperature 230-240 ℃ in the later stage for 4h,and reaction yield was 88%-90% under these conditions.The best process conditions of hydrolysis reaction were: the sulfuric acid concn.of 85%,reaction temperature 70 ℃,reaction time 4h,and the hydrolysis yield was 98.4% under these conditions.The optimal process conditions of Hofmann rearrangement reaction were: reaction temperature 60-70 ℃,reaction time 2h,bromine dosage 16.5-17.0 g.[Conclusion] Under the best process conditions,the yield for 2,6-difluoroaniline synthesized by 2,6-Dichloro-cyanobenzene was up to 68.5%,which was easy to realize industrialization.