In this work, the catalytic capacity of a Mg/Fe layered double hydroxide (LDH) and its mixed oxides to perform Huisgen cycloaddition was studied. The catalytic process was performed in the presence of sodium ascorbate, which was determinant for the success of the 1,3-cycloaddition. The obtained triazoles were evaluated as corrosion inhibitors using electrochemical impedance spectroscopy under static conditions, showing an inhibition efficiency higher than 95% at 50 ppm for some of the triazoles studied. According to the Langmuir isotherm, all the compounds synthesized and analysed exhibit a chemisorption process. Finally, the corrosion process when submerging a steel bar in 1 M HCl was studied using SEM-EDS. This experiment showed that the corrosion process decreases considerably in the presence of 50 ppm of the organic inhibitor.