Disordered meso-macro porous Cu-Ce-Al2O3 nanocomposite (gamma-Al(2-x)M(x)O3 +/- y, M = Cu and or Ce) with different compositions has been synthesized. In situ templated sol-gel method has been adopted with simple EDTA ethylenediamine tetra aceticacid and ethylenediamine molecules to prepare gamma-Al(2-x)M(x)O3 +/- y, (M = Cu and or Ce). Above meso-macro porous materials were characterized by structural, spectroscopy, microscopy and textural techniques. Detailed characterization indicates that Cu2+ ions are introduced into the ceria and alumina lattice positions. Nano composite nature of the gamma-Al(2-x)M(x)O3 +/- y has been confirmed by detailed microscopy investigations. Catalytic activity of the above nanocomposite materials have been screened for environmentally important CO oxidation reaction. 30% Ce-60% Al and 10% Cu containing material shows the best activity among other meso-macroporous material with (50%) 100% CO oxidation at (107 degrees C) 145 degrees C.