This paper describes the optimization of three processes applied in fabrication of a microstructured reactor for complete oxidation of volatile organic compounds. The first process involves the optimization of the electro discharge machining (EDM) method to produce a set of microchannels with a high length to diameter ratio of 100, with a standard deviation from the average diameter below 0.2%, and with a surface roughness not higher than 2.0 µm. To satisfy these criteria, fabrication of microchannels must be carried out with two machining passes in the Al51st alloy. Then, the effect of several parameters on the anodization current efficiency with respect to oxide formation was studied. The best process conditions to get a 30 µm porous alumina layer in a 0.4 M oxalic acid electrolyte, were found to be a temperature of 1 °C, an anodic current density of 5 mA/cm2, and 23 h oxidation time. At last, the resulting coatings were impregnated with an aqueous solution of copper dichromate followed by drying and calcination at 450 °C to produce active catalysts. The effect of a copper dichromate concentration, number of impregnation cycles (1 or 2), and different after-treatments on catalytic activity and stability in complete oxidation of n-butane were studied. The catalytic activity of the obtained coatings is superior to that of alumina supported pelletized catalysts even at much lower loadings of active metals.