The investigation of the thermal behavior of calcium fructoborate samples of composition Ca(C6H10O6BO)2.3.5H2O showed that CaB2O4 is generated as the final solid pyrolysis residue. On the basis of these observations a new, very easy, synthetic procedure for the preparation of high purity samples of this calcium borate is proposed. The material was characterized by X ray powder diffractometry and IR spectroscopy.