Several 2,5-dimethyl-N-substituted pyrroles were prepared by the condensation of different substituted anilines with 2,5-hexanedione using nano lead oxide as an efficient and recyclable catalyst. All the synthesized compounds are confirmed through IR, 1H NMR, 13C NMR and mass spectral data. Nano lead oxide β-PbO (P85) was prepared by dissolving lead acetate dihydrate in 1-propanol at a pH 9.0 under stirring at 85 °C. The structural study and surface morphology of the lead oxide (PbO) were characterized using X-ray diffraction (XRD), Scanning electron microscopy (SEM) and the functional groups of the PbO sample were investigated using infrared spectrophotometer. © 2011 A. Sivakumar.