2H,2H‐COSY and 2H,2H,13C‐RELAY NMR Experiments for the Analysis of Deuteriated Compounds

Determination of the homonuclear coupling between and the correlation of 13C nuclei via vicinal deuterium nuclei has been achieved by 2D NMR spectroscopy. [D5]Pyridine was used to show that the only 0.1‐ to 0.2‐Hz 3J(2H,2H) values lead to significant cross signals in the COSY experiment and that the RELAY experiment is a promising alternative when 2H,13C correlation and 2H,2H COSY NMR spectroscopy fail owing to overlapping of signals.