In this work, the process for production of an ether, 2-methoxy-2,4,4-trimethylpentane (TOME), is investigated using a micro-scale plant with the total holdup of 120 cm(3). This holdup volume is considerably smaller than the conventional pilot plants, which can decrease the operating costs, make the operation easier and improve the safety. The main studied reaction was diisobutylene + methanol producing TOME. Additionally, a side reaction where two molecules of methanol were producing dimethyl ether and water was investigated. The produced TOME was separated from the reactants using a micro-scale horizontal distillation column. The reactants were recycled back to the reactor and the produced TOME was taken out as the product. First, the reactor and the distillation column were characterized separately. Later, the reactor and distillation column were connected together to study the whole process including the recycle stream. The results of the measurements were compared with a dynamic model developed in this work.