High-throughput experimentation enabled by an array-based electrochemical method

Electrochemistry has emerged as a powerful tool to drive chemical transformations. In addition to being an atom-economical approach to chemical synthesis, electrochemistry enables the oxidation/reduction of substrates into desired products at milder reaction conditions than those typically employed in many synthetic organic reactions. Furthermore, electrochemistry allows us access to quantifiable information that can be used to rationally design experiments and optimize reactivity to maximize yield. However, in its native form, electrochemical experimentation is serial in nature, making it quite time-consuming and expensive. This is because the increased parameter space of electrochemical methods means that a dedicated potentiostat/power supply will be required to optimize each reaction condition.
Large arrays of hypothesis-driven, rationally designed electrochemical experiments are powerful tools that overcome the limitations of the currently available electrochemical tools. Using such arrays, chemical and electrochemical parameters relevant to any chemical transformation, whether nanomaterial synthesis or organic electrolysis, can be arrayed to identify optimal conditions. Here, we utilize our multichannel potentiostat (“Legion”) to explore the capability of the array-based electrochemical method for nanomaterial discovery and synthesis and the design and optimization of organic reactions. Legion is integrated with an analytical method for product quantitation, enabling high-throughput electrochemical experimentation. We investigated the parallel electrochemical deposition of palladium nanocubes in different growth environments and identified conditions that produce the desired particle shape and size. Furthermore, using the same array-based approach, we explore the Pd-catalyzed Suzuki-Miyaura cross-coupling reaction in an undivided cell at room temperature.