The biphasic hydroformylation of 1‐octene using a lean aqueous phase as solvent phase for catalyst recycling is discussed here. The gas‐liquid‐liquid reaction was homogeneously catalyzed by industrial standard catalytic system with [Rh(cod)Cl]2 as precursor and TPPTS as ligand. This work summarizes investigations addressing different aspects of the reaction, where a procedural approach was followed to gain understanding of its nature, kinetics and interphase reactivity. Finally, the application of the jet loop reactor is analyzed as a means to intensify the reaction.