Supporting-Electrolyte-Free and Scalable Flow Process for the Electrochemical Synthesis of 3,3′,5,5′-Tetramethyl-2,2′-biphenol,Organic Process Research & Development

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Supporting-Electrolyte-Free and Scalable Flow Process for the Electrochemical Synthesis of 3,3′,5,5′-Tetramethyl-2,2′-biphenol
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2020-06-02 , DOI: 10.1021/acs.oprd.0c00170
Maximilian Selt ₁ , Robert Franke _{2,

3} , Siegfried R. Waldvogel ₁

Affiliation

The most efficient electrochemical synthesis of 3,3′,5,5′-tetramethyl-2,2′-biphenol by dehydrogenative coupling is reported. The electrolysis is performed supporting-electrolyte-free in 1,1,1,3,3,3-hexafluoroisopropanol and at carbon electrodes, whereby glassy carbon electrodes turned out to be superior. To provide sufficient conductivity, pyridine is added, and it can easily be recovered by evaporation and reused. This facilitates the downstream process tremendously, making it simple, economical, and technically viable. The scalability was proven by establishing a flow electrolysis in differently sized narrow-gap flow electrolyzers. Carrying out a multistep cascade electrolysis enabled the challenging hydrogen evolution to be successfully addressed. The scaled-up electrolysis provided an isolated yield of 59% biphenol.

中文翻译：

电化学合成3,3'，5,5'-四甲基-2,2'-双酚的无支撑电解质的可扩展流动工艺

据报道，通过脱氢偶联最有效的电化学合成3,3'，5,5'-四甲基-2,2'-双酚。在1,1,1,3,3,3-六氟异丙醇中和在碳电极上进行无支撑电解质的电解，由此证明玻璃状碳电极是优良的。为了提供足够的电导率，添加了吡啶，可以很容易地通过蒸发将其回收并重复使用。这极大地促进了下游过程，使其简单，经济且在技术上可行。通过在不同尺寸的窄间隙流动电解槽中建立流动电解，证明了可扩展性。进行多步级联电解可以成功解决具有挑战性的氢气释放。放大的电解提供了59％的双酚分离产率。

更新日期：2020-06-02

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