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Quantifying the mass transfer of gas–liquid segmented flow in practical reactions is of significant for the scale‐up design. However, there is a lack of theoretical guidance to predict operational conditions to meet required the mass transfer in a selective dimension‐enlarged microreactor. Herein, the oxidation of 2‐tert‐butyl phenol (2‐TBP) was performed in a selective dimension‐enlarged capillary...