The design and construction of a prototype of a dividing-wall distillation column was possible by integrating previous knowledge in process intensification, energy savings, theoretical control properties, and closed-loop dynamics of thermally coupled distillation sequences. In order to achieve the predicted energy savings for this class of complex distillation column, a dividing wall and a side tank were implemented in order to manipulate the internal flows associated with energy consumption. The reaction between ethanol and acetic acid was conducted within the prototype, and the experimental results indicate that a heterogeneous mixture of ethyl acetate and water is obtained as the top product. The temperature profile measured during the experimental run can be used for controlling the batch distillation column in cyclic operation mode.