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
✍ Scribed by Bernd Wrackmeyer; Christian Köhler
- Publisher
- John Wiley and Sons
- Year
- 1993
- Tongue
- English
- Weight
- 409 KB
- Volume
- 31
- Category
- Article
- ISSN
- 0749-1581
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✦ Synopsis
Abstract
Multinuclear magnetic resonance studies (^1^H, ^13^C, ^15^N, ^31^P) 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 ^1^J(^13^C^1^H) or ^1^J(^15^N^1^H) and on long‐range coupling constants ^2^J(^13^C^1^H), ^2^J(^31^P^1^H), ^3^J(^15^N^1^H), ^3^J(^31^P^1^H) and 2D inverse ^1^H/^15^N 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 ^15^N NMR data are reported, including isotope shifts ^1^Δ^15/14^N(^31^P), obtained by ^31^P INEPT–Hahn–echo extended (HEED) experiments. In the case of the monomeric iminophosphane 2, the largest negative value ^1^Δ^15/14^N(^31^P) = −144 ppb was observed. Absolute signs of numerous coupling constants across one to five bonds were determined, involving the NMR active nuclei ^1^H, ^13^C, ^15^N, ^19^F and ^31^P.