Formation of azeotropic mixtures may cause difficulties in separation. Synthesis and isolation of methyl acetate is a representative example for formation of azeotropic product mixtures. In this project chemical reaction engineering in batch and plug flow reactor, as well as the combination of synthesis with extractive isolation of methyl acetate from the multi component mixture methanol/acetic acid/methyl acetate/water, were investigated. Reaction paths were discussed in order to avoid or bypass the low boiling azeotropic mixtures of methyl acetate with water and methanol. The esterification reaction was heterogeneously catalyzed with cation exchange resins. For extractive separation of methyl acetate aliphatic hydrocarbons of the C-8 to C-10 class were used. The project provides the basic strategy for process design of esterification processes. In the concept of process intensification, alternative process routes in methyl acetate synthesis and isolation were discussed.