The aim of this research is, to clarify which route the sol-gel-process is taking in the case of a Al-Mg-spinel slurry, in particular, whether the hydrolysis reaction or the spinel formation is faster and which of the intermediate hydroxide phases Al(OH)3, and Mg(OH)2, or MgO and Al2O3 or MgAl2O4H2O are formed during the spinel formation. The spinel-alloy was produced using the polymeric route during wet chemical processing. Aluminium-isopropoxide was hydrolyzed in order to form the boehmite-sol and then the same amount of magnesia was added and mixed. This sol precipitated as boehmite (AlOOH) and brucite (Mg(OH)2) after ageing for 12h as confirmed by differential thermal analysis (DTA), and differential thermal gravity (DTG) measurements. After that, the powders were subsequently annealed at 900oC for 3h in air and observed by TEM. Calculations using thermodynamic enthalpy data are in good agreement with the experiments and can be used to predict reaction paths in other system as well.