CO adsorption on β-zeolite with highly dispersed CuCl2 · 2H2O was studied by IR spectroscopy. The results of XRD and 29Si NMR indicate that CuCl2 · 2H2O is highly dispersed into β-zeolite channel as a monolayer. The IR spectra of adsorbed CO on the zeolites demonstrate that two distinct types of adsorption sites exist in the zeolites, i.e., cation and non-cation exchange sites. Two simultaneous processes, solid phase ion-exchange and molecular diffusion, are involved in the dispersion of CuCl2 · 2H2O.