One-pot nanocrystalline mesoporous MgOZrO 2 solid solution was synthesised by a simple evaporation induced self assembly route with ZrO(NO 3 ) 2 Á8H 2 O and Mg(NO 3 ) 2 Á4H 2 O as precursors along with triblock copolymer of Pluronic P123 as structure directing agent. The prepared catalysts were characterised by X-ray diffraction studies (XRD), N 2 adsorption/desorption isotherms, Fourier transform infrared spectroscopy, TPD of CO 2 and transmission electron microscopy (TEM). XRD results confirm the formation of nanocrystalline ordered mesoporous structure of MgO-ZrO 2 (MZx). Additionally the TEM and N 2 sorption study confirms the ordered mesoporous nature of MZx materials. The Mg 2? incorporation into zirconia lattice presumably stabilizes the tetragonal phase and avoids excessive growth of zirconia crystals. The activity of the prepared samples was tested for the transesterification of glycerol. Among all tested, the MZ2 catalyst (Mg:Zr ratio 1:2) proved to be efficient for the transesterification of glycerol by dimethyl carbonate (96 % conversion and 88 % yield). We attribute the high efficiency of MZ2 to its basic nature and highly dispersed MgO species.