Aseries of hybrid heteropoly acids (HPA) were prepared. The HPA/NaY and HPA/NaY/MCM-41 hybrids of the synthesized catalysts were characterized using XRD, BET, TGA, SEM and FT-IR techniques. The results show that reasonable amount of HPA in HPA/NaY and HPA/NaY/MCM-41 hybrids remains even after washing with water, which indicates that heteropoly anions were strongly bonded to the porous materials. The catalytic properties of the hybrid catalysts were examined for the preparation of 2-(4- nitrophenyl)-2,3-dihydro-1H-perimidine. The yield for perimidine by different catalysts was in order of HPA/NaY > HPA/NaY/MCM-41 > NaY > HPA > MCM-41.