The electrochemical reduction of alpha-diketones and alpha-diimines with the tritosylate of diethanolamine produces the corresponding aza crown compounds. This study was conducted using cyclic voltammetry in an aprotic medium and by preparative electrolysis on a stirred mercury pool. The obtained products were fully characterized by spectroscopic IR, NMR and HRMS methods and by elementary analysis. (C) 2016 The Electrochemical Society.