Thermal decomposition of aluminum isopropoxide in toluene at 315degreesC resulted in chi-alumina that had high thermal stability, whereas the reaction at lower temperatures resulted in formation of an amorphous product. The chi-alumina thus obtained directly transformed to alpha-alumina at similar to1150degreesC, bypassing the other transition alumina phases,whereas the amorphous product transformed to gamma-alumina and then to theta-alumina before final transformation to alpha-alumina. When the chi-alumina, solvothermally synthesized at 315degreesC, was recovered by the removal of the solvent at the reaction temperature, thermal stability of the product was improved further. This procedure is convenient because it avoids bothersome work-up processes that yield large-surface-area and large-pore-volume alumina.