The use of carbon monoxide to produce organic compounds is an important research area for the future. In particular the carbon monoxide coupling reaction takes place at moderate reaction conditions,with low consumption of energy, to produce oxalic acid and oxalate. The chemicals are feedstocks for ethylene glycol synthesis by hydrogenation of oxalate, as well as for products such as pesticides, pharmaceuticals, foodstuffs, polymers, and fine chemicals. The carbon monoxide coupling reaction on supported metal catalysts Pd/Al{sub 2}O{sub 3} and Pd-Fe/Al{sub 2}O{sub 3} was used to study the characteristics of the catalyst under different conditions. The results indicated that the catalytic activation temperature influenced the catalytic activity and that there was an optimum activation temperature. The characteristics of effective coupling catalysts were found to be smaller surface areas and bigger pores, for example the {alpha}-phase of aluminum oxide. X-ray photoelectron spectroscopic analysis results show that the catalytic reaction of CO coupling occurs via a redox mechanism.