Calcium monoaluminate was synthesized by the sol–gel method and the effect of europium and neodymium oxides on the synthesis and structuring kinetics was studied in the temperature range 500 – 1000°C. It was determined that the formation of the structure of calcium monoaluminate occurs at 1000°C and with exposure for 4 h of a xerogel obtained based on a mixture of Al(NO3)3 + Ca(NO3)2 at a compound ratio of 2 : 1, respectively. In the sample obtained, the intermediate mineral is mayenite Ca12Al14O33. With the introduction of the mineralizing europium oxide Eu2O3 in an amount of 1.5 wt.% greater than 100 wt.% in Al(NO3)3 + Ca(NO3)2 composition, at a synthesis temperature of 1000°C, the exposure time for maximum formation of calcium monoaluminate is reduced to 1 h. In samples containing Nd2O3, for the maximum formation of calcium monoaluminate at the same exposure time, it is necessary to introduce it in an amount of 5 wt.%.