Natural mesolite type zeolite was collected, modified by sulphuric acid treatment and characterized by using Powder-X ray diffraction, Scanning electron microscopy and Energy dispersive spectroscopy, Fourier transform infrared spectroscopy. Temperature programmed ammonia desorption, BrunauerEmmer-Teller surface area analysis. Modified dealuminated mesolite shows an efficient catalytic activity for one pot synthesis of 3-methyl-4-arylmethylene-isoxazol-5(4H)-ones derivatives, via one pot three component condensation of benzaldehyde, ethylacetoacetate and hydroxylamine hydrochloride. Present method offers several advantages over the reported methods like a simple and inexpensive modification of catalyst, mild reaction condition, easy separation of catalyst, simple work-up procedure, nonchromatographic isolation and purification desired product and excellent yield. Furthermore, catalyst could be reused without significant loose in activity.