Technical note: Unequivocal identification of 5-methoxy-DiPT with NOESY NMR and GC-IRD

•NOESY NMR.•GC-IRD.•Tryptamine.•5-MeO-DiPT. The need for new analytical methods to differentiate isomers and closely related compounds have become increasingly important due to the fast evolution of new psychoactive substances. 2D NMR and GC-IR spectroscopies are promising techniques due to their capabilities to differentiate isomers. This case study highlights specifically the use of Nuclear Overhauser Effect Spectroscopy (NOESY) and solid deposition GC-IRD in the unequivocal identification of 5-methoxy-DiPT, a tryptamine analogue.