Reactive distillation (RD) is an integrated operation combining both reaction and separation, thus improving the productivity and selectivity, reducing the energy usage, eliminating the need for solvents and leading to intensified highly-efficient systems. In previous work, we performed the conceptual design and modeling of a reactive distillation process for synthesis of unsaturated polyesters. The simulation results of our previous work clearly demonstrated that reactive distillation is a promising alternative for the polyesters synthesis. This paper presents our pilot scale experimental validation work on the proposed RD process for polyester synthesis. Two configurations are investigated: (1) a RD column alone and (2) a RD column couple...