Abstract The efficiency of two‐dimensional homonuclear 1 H 1 H NOE spectroscopy in characterizing and fully assigning the 1 H NMR spectra of several isomers of meso ‐ or ring‐substituted deuteroporphyrins is demonstrated. The carbon resonances of the skeleton and the substituents were fully assigned using two‐dimensional reverse heteronuclear shift correlation spectroscopy.