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We present a reconfigurable flow chemistry strategy for facile transition between accelerated screening and continuous synthesis of linear aldehydes through homogeneous rhodium-catalyzed hydroformylation of alkenes. The intensified mass and heat transport rates of the utilized membrane-based flow reactor enable access to safe and desirable reaction conditions (i.e., 50 psig syngas pressure) while providing high chemoselectivity and regioselectivity of the produced aldehydes. Additionally, by conducting hydrogen–deuterium scrambling experiments, we propose a reaction mechanism for the highly efficient hydroformylation reaction in flow.