Continuous-Flow Process for the Synthesis of m-Nitrothioanisole

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• 作者：Zhiqun Yu ; Xiaoxuan Xie ; Hei Dong ; Jiming Liu ; Weike Su
• 刊名：Organic Process Research & Development
• 出版年：2016
• 出版时间：April 15, 2016
• 年：2016
• 卷：20
• 期：4
• 页码：774-779
• 全文大小：344K
• 年卷期：0
• ISSN：1520-586X

文摘

A continuous-flow process for the preparation of m-nitrothioanisole has been set up. The starting material m-nitroaniline was diazotized to give diazonium chloride, followed by azo-coupling with sodium thiomethoxide to give 1-(methylthio)-2-(3-nitrophenyl)diazene, then dediazoniated to gain m-nitrothioanisole in high yield. The continuous-flow process minimized accumulation of the energetic intermediate diazonium salt and has a better capacity for adapting large-scale production. A solvent was introduced in the azo-coupling section to create a biphasic flow system. Side products were inhibited eminently in this flow process.