A High-Output, Continuous Selective and Heterogeneous Nitration of p-Difluorobenzene

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• 作者：Zhiqun Yu ; Yanwen Lv ; Chuanming Yu ; Weike Su
• 刊名：Organic Process Research & Development
• 出版年：2013
• 出版时间：March 15, 2013
• 年：2013
• 卷：17
• 期：3
• 页码：438-442
• 全文大小：273K
• 年卷期：v.17,no.3(March 15, 2013)
• ISSN：1520-586X

文摘

A practical continuous nitration process for 2,5-difluoronitrobenzene via nitration of p-difluorobenzene with fuming nitric acid in 98% yield has been developed. The excellent yield of this liquid/liquid biphasic reaction resulted from the advantages of a continuous flow system. The 2.0 equiv sulfuric acid could be used three times directly with product yields in the range of 96鈥?8%, and further recycling of waste acid could be partly achieved by adjusting the concentration of sulfuric acid. Reaction time could be brought down to 2 min by increasing the reaction temperature and thereby taking advantage of superior mass and heat transfer of this continuous flow system.