Abstract. Rapid synthesis of poly[(pyrrole-2,5-diyl)-co-(benzylidene)] was achieved under microwave irradiation via the condensation of pyrrole and benzaldehyde in 1,2-dichloroethane using acid exchanged montmorillonite clay called Maghnite-H + (Mag-H + ) as an efficient catalyst. The effect of the amount of catalyst and of time on the polymerization yield and on the viscosity of the polymers was studied. Compared with conventional static interfacial polymerization, the microwaveradiation polymerization reaction proceeded rapidly and was completed within 35 s. The conjugated polymer was characterized by means of 1 H-NMR, X-ray diffraction, FT-IR spectroscopy and AFM. The X-ray data showed the presence of a backbone form of the [(pyrrole-2,5-diyl)-co-(benzylidene)] formed.