Mesoporous gamma-aluminas (γ-Al 2 O 3 ) were synthesized starting from an unusual precursor of polyoxohydroxide aluminum (POHA). This precursor was obtained from aluminum oxidation in alkaline water-ethanol solvent in the presence of d-glucose that induces the formation of a gel, which leads to the POAH powder after ethanolic treatment. Precipitated POHAs were calcined at different temperatures (300, 400, 700 and 900 °C) resulting in the metastable γ-Al 2 O 3 phase. Whereas at 300 °C no γ-Al 2 O 3 phase was formed, unexpectedly, mesoporous γ-Al 2 O 3 was obtained at 400 ºC having a high specific surface area (282 m 2 /g) and a narrow pore size distribution. At higher temperatures, the aluminas had the expected decrease in surface area: 166 m 2 /g (700 °C) and 129 m 2 /g (900 °C), respectively. The structural change from POHA to alumina calcined at 400 ºC occurs directly without the need to isolate the hydroxide or oxyhydroxide aluminum precursors. Both POHA and transition aluminas were characterized by Fourier Transform Infrared spectroscopy (FTIR), X-ray diffraction (XRD), N 2 sorption and Scanning Electron Microscopy (SEM). These findings show an alternative route to produce high standard aluminas.