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Abstract Within the realm of drug discovery, high‐throughput experimentation techniques enable the rapid optimization of reactions and expedited generation of drug compound libraries for biological and pharmacokinetic evaluation. Herein we report the development of a segmented flow mass spectrometry‐based platform to enable the rapid exploration of photoredox reactions for early‐stage drug discovery. Specifically, microwell plate‐based photochemical reaction screens were reformatted to segmented flow format to enable delivery to nanoelectrospray ionization‐mass spectrometry analysis. This approach was demonstrated for the late‐stage modification of complex drug scaffolds, as well as the subsequent structure–activity relationship evaluation of synthesized analogs. This technology is anticipated to expand the robust capabilities of photoredox catalysis in drug discovery by enabling high‐throughput library diversification. 

An experiment designed to teach principles of continuous flow technologies for photocatalysis is 10 described as a part of a two-week summer camp program for high school students. Students learned about green chemistry, photocatalysis, flow chemistry, and the role of 3–D printing for the design and production of custom millifluidic reactors. Students examined reactor designs which differed in terms of residence times and mixing capabilities. Such evaluation was based on the combination of blue and yellow dyes, followed by running a photocatalytic thiol-ene reaction on gram-scale.