Due to decreasing oil resources, alternative fuels such as biodiesel are required. The nanomagnetic catalyst CaO/NaY-Fe3O4 was synthesized and used for biodiesel production from canola oil. The structure of the catalysts was characterized by X-ray diffraction, field emission scanning electron microscopy, Brunauer-EmmettTeller method, Fourier transform infrared spectroscopy, and vibrating sample magnetometer method. To optimize the influence of the operating variables, such as the methanol/canola oil molar ratio, the amount of catalyst, and the reaction time, on the yield of transesterification reaction, an experimental design was applied based on the Box-Behnken method. The optimum values of these variables were predicted by the cubic model and were in excellent agreement with the experimental results.