This article reports the esterification of lauric acid and methanol studied using a thermally coupled distillation sequence with a side rectifier and the Petlyuk distillation column. The product of the esterification can be used as biodiesel. It was found that the thermally coupled distillation sequence with a side rectifier can produce ester with a high purity (around 0.999) and also pure water, and the excess of methanol is recovered in the side rectifier. The results indicate that the energy requirement of the complex distillation sequence with a side rectifier can be reduced significantly by varying operational conditions. These reductions in energy requirements can be interpreted as reductions in carbon dioxide emissions. Moreover, dynamic tests for control of the composition of the ester and control of two temperatures for the thermally coupled distillation sequence with a side rectifier indicate that it is possible to eliminate disturbances in the feed composition, while the composition of the biodiesel remains at the desired value.