The aim of this work is basically centred in the improvement of the obtention of the peroxides precursors of macrocyclic lactones (C-11 and C-16) through the Story synthesis useful as raw materials for high performance linear polyesters. As a starting point, the yield has been increased respect to the classic synthesis using mild and intrinsically safer reactants. Concretely, a yield of 65% in triperoxide of cyclohexanone has been achieved using 35% hydrogen peroxide and phosphotungstic acid as catalyser. For this intention two factorial experimental designs, fractional and complete, have been carried out. The analytical method adequate for the reactive system studied (HPLC-UV-RI) has been chosen as well as the optimal operating conditions. A quantification of the risk on the first part of the reaction in calorimetric terms has been performed. The techniques employed have been reaction calorimetry and DSC.