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Despite many recent efforts, the field of organic electrosyn‐thesis faces important challenges due to the intricate nature of heterogeneous redox processes, the wide parameter space to be explored and the lack of standardized methods. To overcome these limitations, we developed a cost‐effective high‐throughput electrochemical (HTE) reactor capable of running 24 individually controlled parallel reactions. This system allows the rapid testing of electrochemical parameters on a given reaction, assessing not only yield but also reproducibility. Using the hypervalent iodine‐mediated dearomatization of phloretic acid as a demonstration of HTE capabilities, we ran more than 200 electrosyntheses in different experimental conditions and demonstrate the effect of parameters such as total charge transferred, current, electrode materials, electrolyte formulation and concentration, mediator formulation and concentration and electrochemical technique of oxidation. Notably, this report demonstrates that while catalytic amounts of iodine mediator can be used successfully, the reproducibility may be affected, which calls for a cautious approach when developing similar transformations. Using cyclic voltammetry, density functional theory, chronopotentiometry, and Raman spectroscopy, we shed light on the causes of this issue. [ABSTRACT FROM AUTHOR]

The front cover of the journal ChemElectroChem showcases the potential of high-throughput electrosynthesis, with a researcher collecting the products with the highest yield. This method offers the opportunity to accelerate research by optimizing existing reactions and discovering new pathways. The cover is associated with a research article by Eric McCalla, Janine Mauzeroll, and their colleagues, which provides more information on this topic. [Extracted from the article]

Mussel byssus offers bio‐inspired designs for advanced adhesives, coatings, and supramolecular hydrogels. Solidification of secreted proteins into mechanically robust fibers is triggered by a pH jump from acidic fluid condensates to basic seawater conditions driving protein crosslinking by metal coordination with 3,4‐dihydroxyphenylalanine (DOPA). Knowledge of the dynamic and localized pH changes during secretion is currently lacking. Yet, this information is crucial for controlling the gelation and properties of mussel‐inspired DOPA‐modified materials. Here, an iridium oxide‐based pH microsensor combining high mechanical stability and spatial resolution is used to measure the acidic pH during byssus secretion and to map mussel‐inspired hydrogels revealing compositional heterogeneity resulting in mechanically distinct regions. Within the hydrogel, high pH values >12 are measured which are detrimental to DOPA due to its strong propensity for oxidation, which adversely alters gel properties. This demonstrates the need to improve preparation methods of mussel‐inspired adhesive materials to more closely mimic native processes. [ABSTRACT FROM AUTHOR]