Ultrasound-assisted approach was successfully applied for the synthesis of mayenite from calcium and aluminum hydroxides and then subsequently impregnated with Ni by the wet impregnation method. The synthesis was performed with a 13mm probe-type ultrasound, operating under an acoustic power of 30.5W and a frequency of 20kHz. Ultrasound application was studied in detail from a 3k experimental design, where the variables studied were ultrasound time (10-50min) and calcination temperature (900-1200°C). Ultrasound promoted an effective dispersion of the precursors in a short time of 10min leading to a high conversion to mayenite after calcination at 1200°C. Ultrasound treatment also had a positive effect on Ni impregnation, increasing the dispersion of the metal in the support and leading to a stronger interaction of nickel-containing species with mayenite support. The use of ultrasound application has proved to be attractive both for catalyst properties and for facilitating catalyst synthesis.