The "Green" Electrochemical Synthesis of Periodate
The "Green" Electrochemical Synthesis of Periodate
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DOI：
10.1002/anie.202002717
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发表时间：
2020-04-15
影响因子：
16.6
通讯作者：
Waldvogel, Siegfried R.
中科院分区：
文献类型：
--
作者：
Arndt, Sebastian;Weis, Dominik;Waldvogel, Siegfried R.
高级高碘酸盐相对昂贵，但对于许多敏感应用如活性药物成分的合成是必需的。这些高成本源于在当代电化学方法中使用二氧化铅阳极以及昂贵的起始材料。报道了一种由碘化物直接电化学合成高碘酸盐的方法，该方法成本低，原料易得。氧化是在硼掺杂的金刚石阳极，这是耐用，无金属，无毒进行。避免二氧化铅最终降低了净化和质量保证的成本。通过统计方法优化了电解过程，并在电解流动池中放大，通过环化方案提高了时空产率。建立了一种LC-PDA分析方案，能够同时以显着的精度简单地定量碘化物、碘酸盐和高碘酸盐。
High-grade periodate is relatively expensive, but is required for many sensitive applications such as the synthesis of active pharmaceutical ingredients. These high costs originate from using lead dioxide anodes in contemporary electrochemical methods and from expensive starting materials. A direct and cost-efficient electrochemical synthesis of periodate from iodide, which is less costly and relies on a readily available starting material, is reported. The oxidation is conducted at boron-doped diamond anodes, which are durable, metal-free, and nontoxic. The avoidance of lead dioxide ultimately lowers the cost of purification and quality assurance. The electrolytic process was optimized by statistical methods and was scaled up in an electrolysis flow cell that enhanced the space-time yields by a cyclization protocol. An LC-PDA analytical protocol was established enabling simple quantification of iodide, iodate, and periodate simultaneously with remarkable precision.