A special, efficient and reusable heterogeneous catalytic system is reported for the one-pot three-component synthesis of a series of malonamide and 2,3,4,5-tetrahydrobenzo[b] [1,4]oxazepine derivatives in the presence of a heterogeneous material composed of MCM-48/H 5 PW 10 V 2 O 40 in aqueous media and at room temperature. The products were identified using physical data (melting points) by comparison with those reported in the literature. Also, the structures of the new compounds were characterized by means of infrared, 1 H NMR, 13 C NMR and CHN analyses.