Aluminum acetylacetonate, Al(acac)(3), was prepared in the reaction between the mineral boehmite, [AlO(OH)](n), and acetylacetone (2,4-pentanedione; Hacac) in water. In this one-step synthesis, the pale yellow crystalline product precipitated out of the solution. Characterization of the recrystallized crystal by mass spectrometry, thermogravimetric/differential thermal analysis (TG/DTA), (HNMR)-H-1, and the X-ray diffraction (XRD) was consistent with Al(acac)(3). This is the first example of the preparation of the six-coordinate aluminum compound from boehmite.