Abstract: The hydrolysis of aluminum-tri-(sec-butoxide), ASB, in ionic and nonionic media is shown to be a useful method for the synthesis of aluminum minerals. Infrared and X-ray analysis were used to identify the reaction products. Pseudoboehmite is formed at low water to aluminum ratios. At higher water content, transformation of pseudoboehmite occurs with bayerite as the final phase. Dawsonite-type minerals are produced when ASB is hydrolyzed in the presence of sodium, potassium, or ammonium bicarbonate. Infrared evidence suggests that the carbonate group is more perturbed than indicated by the proposed crystal structure. A compound with a structure like the pyoaurite-sjögrenite group was obtained when ASB reacted with a lithium carbonate solution. The infrared spectrum indicates the possible existence of bicarbonate and carbonate ions between the brucite-like layers.