1 H and 13 C NMR analyses of amiodarone, desethylamiodarone and desoxoamiodarone

The 1 H and 13 C NMR spectra of amiodarone, a potent cardiac antiarrhythmic agent, desethylamiodarone, the main metabolite of amiodarone and desoxoamiodarone, a less toxic form of amiodarone, were assigned using a combination of NMR techniques. Methods applied include 1 H‐ 1 H COSY, homonuclear Hartmann–Hahn relayed spectroscopy (HOHAHA), broadband decoupled 1 H– 13 C chemical shift correlation, long‐range 1 H– 13 C chemical shift correlation and selective INEPT. This combination of NMR experiments has completed a molecular walk along the covalent framework of the cardiac drug molecules, and removed ambiguities in their 1 H and 13 C NMR assignments.