AbstractT‐2 toxin dissolved in CDCl3and C6D6and T‐2 triol in CDCl3were studied by 1D and 2D n.m.r. spectrometric methods. Comprehensive n.m.r. spectral parameters are reported. Iterative analysis of the isovaleroxy proton resonances of T‐2 toxin in C6D6and T‐2 triol in CDCl3was carried out. The assignments of the proton and carbon resonances of the ace‐toxy groups and of the H‐13 and H‐15 resonances of T‐2 toxin are given. The known conformation of the trichothecene ring system was con