Aluminum ethoxide (AE) was synthesized to a high purity grade through dissolution reaction and vacuum distillation from used Al cans (UACs) under the condition of 3 mol C2H5OH/mol Al of stoichiometric ratio. 10.3 mol HgI2/mol Al as a catalyst and 0.5 mol xylene/mol Al as a solvent for the control of reaction temperature were added. The UACs were cut into small pieces and heat-treated at the condition of 600 ℃ to remove impurities from UACs. Using the pretreated UACs, the high purity AE was synthesized and analyzed quantitatively by a complexometric method. The results of our experiment revealed that the reaction gives a 99.1% purity and 75% yield corresponding to the total amount of Al existing in the pretreated UACs.