Aminophenol compounds are usually employed in coordination chemistry due to their versatility to form metal complexes. Heptadentate N₅O₂ aminophenol ligands can lead to the obtention of lanthanoid complexes with pentagonal bypiramidal (pbp) geometry, which are very interesting in the field of molecular magnetism. In this communication we report an optimised method for obtaining two similar N₅O₂ aminophenols named 2-((((6-(((5-hydroxy-2-R-benzyl)(pyridin-2-ylmethyl)amino)methyl)pyridin-2-yl)methyl)(pyridin-2-ylmethyl)amino)methyl)-4-R-phenol (R = methyl or methoxy), which significantly improves the few examples of synthesis of this type of compound reported in literature.