Zeolites with MWW topology (MCM-22, ITQ-2, and MCM-36) exchanged with copper and iron were studied as catalysts for selective catalytic reduction of NO with ammonia. It was shown that delamination and pillaring of layered MCM-22 zeolite resulted in the formation of ITQ-2 and MCM-36, respectively. Both these materials were characterized by MWW topology and significant contribution of mesopores. In a series of the zeolite based catalyst the most promising results in a process of selective catalytic reduction of NO with ammonia were obtained for the copper doped samples (Cu-MCM-22 and Cu-ITQ-2), however catalytic performance of the studied catalytic systems strongly depends on type, content and form of deposited transition metal species. Moreover, both these catalysts were found to be catalytically stable in the DeNOx process after hydrothermal treatment.