These pyrophoric organoaluminum liquids are very ef‘cient catalysts in a wide variety of polymerization reactions and also have found use as hydrogenation initiators (e.g., formation of NaAlH4 or AlEt2H under pressure from the elements [5,6]). Because these compounds ignite spontaneously on contact with oxygen or moisture, there are restrictions on their transportation. Here, a simple method for their preparation in the laboratory is presented based on several procedures reported in the literature, which have been adapted to save time, simplify apparatus, and in certain cases improve the yield.