Abstract. The study of non-hydrolytic reactions for the synthesis of Mg x Al 2(1−x) Ti (1+x) O 5 solid solution with x = 0.6 is reported. The reagents chosen were Al(OsBu) 3 , Ti(OiPr) 4 , TiCl 4 and Mg(NO 3 ) 2 ·6H 2 O in toluene. The reactions were followed using 13 C Nuclear Magnetic Resonance (NMR) spectroscopy. Sol-gel synthesized powders were calcined in air at 300, 500, 1000, and 1200• C for 1 h. The powders were analysed by X-Ray Diffraction (XRD) demonstrating the formation of a Mg 0.6 Al 0.8 Ti 1.6 O 5 phase in samples treated at the higher calcination temperature.