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Dimethyl, diethyl, and di‐iso‐butyl aluminum acetylacetonate compounds were synthesized to deposit Al2O3thin films by low‐pressure metal–organic (LP‐MO)CVD. Alumina films were grown in the temperature range 400–520 °C under an oxygen or water vapor atmosphere. A kinetic model was applied to analyze the experimental data and to compare the properties of the three precursors. The model, supported by in‐line Fourier transform infrared (FTIR) measurements, clearly distinguished the rate‐determining steps of the heterogeneous process, with kinetic constants correlated to the molecular structure of the precursors. A method of optimizing deposition conditions, on the basis of the uniformity of the obtained thin films, is discussed.