Multinuclear (1H, 13C, 15N, 19F, 31P) one‐ and two‐dimensional magnetic resonance study of tert‐butylamino‐tert‐butyl‐fluorophosphane, tert‐butylimino‐tert‐butylphosphane and of its dimer formed by [1 + 2] cycloaddition

Abstract

AbstractMultinuclear magnetic resonance studies (1H, 13C, 15N, 31P) of three phosphorus–nitrogen compounds [tert‐butylamino‐tert‐butylfluorophosphane (1), tert‐butylimino‐tert‐butylphosphane (2) and its dimer (3)], in which numerous one‐ and two‐dimensional NMR experiments [heteronuclear shift correlations based on 1J(13C1H) or 1J(15N1H) and on long‐range coupling constants 2J(13C1H), 2J(31P1H), 3J(15N1H), 3J(31P1H) and 2D inverse 1H/15N correlations] were used, led to consistent assignment of the NMR spectra. By this means, incorrect data in the literature were corrected for 1 and 3 and new 15N NMR data are reported, including isotope shifts 1Δ15/14N(31P), obtained by 31P INEPT–Hahn–echo extended (HEED) experiments. In the case of the monomeric iminophosphane 2, the largest negative value 1Δ15/14N(31P) = −144 ppb was observed. Absolute signs of numerous coupling constants across one to five bonds were determined, involving the NMR active nuclei 1H, 13C, 15N, 19F and 31P.