Catalytic distillation experiments were designed and carried out in a pilot-scale column to prove the technical feasibility of the heterogeneously catalyzed n-propyl propionate synthesis by esterification of propionic acid with 1-propanol using the surface-sulfonated ion-exchange resin Amberlyst 46. The experiments cover a broad range of decisive operational parameters, for example, reflux ratio, column load, distillate-to-feed ratio, and molar feed ratio of the reactants. The reconciled results comprise a complete set of concentration and temperature profiles along the column height and, hence, exhibit detailed and reliable data for model validation purposes.