COORDINATION POLYMERS (CPS) ARE INFINITE SYSTEMS CONTAINING METAL IONS AND ORGANIC LIGANDS LINKED VIA COORDINATION BONDS AND OTHER WEAK CHEMICAL BONDS. THEY HAVE RECEIVED SIGNIFICANT ATTENTION FOR THEIR STRUCTURAL AND DIVERSE APPLICATIONS, SUCH AS MAGNETISM, SORPTION, ELECTRICAL CONDUCTIVITY, LUMINESCENT SCIENCE AND CATALYSIS. POLYOXOMETALATES (POMS) ARE ALSO KNOWN DUE TO THEIR VARIOUS TOPOLOGICAL PROPERTIES AND APPLICATIONS IN CATALYSIS. THEY HAVE BEEN WIDELY UTILIZED AS INORGANIC BUILDING BLOCKS FOR THE CONSTRUCTION OF ORGANIC-INORGANIC HYBRID MATERIALS [1]. THE KNOEVENAGEL CONDENSATION REACTION IS ONE OF THE MOST USEFUL METHODS FOR CARBON–CARBON BOND FORMATION. IT HAS BEEN WIDELY USED FOR THE PREPARATION OF A RANGE OF SUBSTITUTED ALKENES, COSMETICS, PERFUMES AND PHARMACEUTICAL INDUSTRY. CONVENTIONALLY, KNOEVENAGEL CONDENSATION REACTIONS PROCEED HOMOGENOUSLY IN THE PRESENCE OF VARIOUS BASE CATALYSTS. UNFORTUNATELY, THE HOMOGENEOUS CATALYSIS COULD NOT SOLVE THE PROBLEM IN SEPARATION AND RECYCLING OF CATALYST. FOR THIS REASON, HETEROGENEOUS CATALYSTS HAVE BEEN USED IN KNOEVENAGEL CONDENSATION [2-3].IN THIS WORK, THE [CUI(4,4´-BIPY)]3[PMO10 VIMO2 VO40{CUII(2,2´-BIPY)}] WAS PREPARED USING COPPER SALT, 4,4´-BIPYRIDINE, 2,2´-BIPYRIDINE AND HETEROPOLYACID UNDER HYDROTHERMAL CONDITION. THE CATALYST WAS IDENTIFIED USING XRD, FT-IR AND ATOMIC ABSORPTION. THEN IT WAS USED AS HETEROGENEOUS CATALYSTS FOR KNOEVENAGEL CONDENSATION REACTION (FIG.1). IN THIS STUDY, FACTORS SUCH AS INFLUENCE OF REACTION TEMPERATURE, TIME, AMOUNT OF CATALYST, SOLVENT AND SUBSTITUTENTS OF ALDEHYDES AND MALONONITRILE HAS BEEN CONSIDERED. AFTER OPTIMIZED THE REACTION CONDITIONS, IT WAS FOUND THAT AT 60˚C IN ETHANOL WITHIN 4H, 100% CONVERSION TOWARDS THE FORMATION OF KNOEVENAGEL CONDENSATION PRODUCTS IS CONSIDERABLE.