The reactive dividing-wall column (RDWC) presents a highly integrated process that enables significant reductions in investment costs and energy consumption. However, the high degree of integration of this apparatus causes numerous interactions between kinetics, vapor-liquid equilibrium, and mass transfer. To ensure a reliable operation of the RDWC, suitable control schemes need to be developed and experimentally validated. A decentralized control scheme for the RDWC is presented and for the first time experimentally investigated on an RDWC pilot plant. A comparison of experimental and simulated data is carried out and shows good agreement.The transesterification of n-butyl acetate with 1-hexanol (Eq. (1)), catalyzed by the immobilized enzyme Novozym 435, is selected as reference system. A detailed investigation of the