Efficient ozonolysis of steroids via electrochemical ozone production coupled with microchannel reactor

Abstract Ozonolysis offers a clean and selective route for CC bond cleavage, but conventional processes suffer from ozonide explosion hazards and poor mass transfer. Here, we integrate electrochemical ozone production (EOP) with continuous‐flow microchannel ozonolysis for the safe conversion of steroid substrates. A dual surfactant modified β‐PbO 2 electrocatalyst (β‐PbO 2 ‐CP) in a self‐developed ozone electrolyzer achieved high ozone generation efficiency with over 750 h stability. Precision‐engineered microchannel reactor intensified gas–liquid transfer via microscale bubble dynamics, affording 91.3% conversion and 98.1% selectivity for 17α‐methyltestosterone, which achieved a 33.7‐fold increase in space–time yield vs. batch reactor. Computational fluid dynamics (CFD) simulations revealed electrothermal flow modeling showed 42.6% lower peak temperature with 98.9% prediction accuracy in the ozone electrolyzer and elucidated gas–liquid behavior in microchannel reactor. This integrated platform demonstrates a controlled continuous‐flow approach suitable for pharmaceutical manufacturing, highlighting the potential of coupling EOP with flow chemistry for industrial oxidative processes.