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14N and 15N NMR spectroscopic characterization and analysis of cyclic sulfur imides

✍ Scribed by Tristram Chivers; Mark Edwards; Deane D. McIntyre; Kenneth J. Schmidtt; Hans J. Vogel


Publisher
John Wiley and Sons
Year
1992
Tongue
English
Weight
467 KB
Volume
30
Category
Article
ISSN
0749-1581

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✦ Synopsis


Abstract

The ^14^N and ^15^N NMR spectra of natural abuadance and ^15^N‐enriched samples of S~7~NH and S~4~(NH)~4~ were obtained by direct detection and by a variety of polarization transfer techniques. Sensitivity enhancements of ca 10 (compared with direct detection) for the INEPT pulse sequence and ca 100 for the HMQC (heteronuclear multiple quantum coherence) + BIRD (bilinear rotation decoupling) sequence were observed for the imides. ^15^N spin–lattice relaxation constants (T~1~) of 10.2 Β± 0.1 and 12.6 Β± 0.1 s were determined for S~7~NH and S~4~(NH)~4~, respectively. The HMQC procedure was used to obtain the ^15^N and ^1^H NMR chemical shifts and ^1^1__J__(^15^N, ^1^H) values for 1,3‐,1,4‐ and 1,5‐S~6~(NH)~2~, 1,3,5‐ and 1,3,6‐S~5~(NH)~3~. The trends in NMR chemical shifts and coupling constants are discussed in the context of the known molecular structurts of cyclic sulfur imides. The use of NMR techniques for the analysis of mixtures of cyclic sulfur imides is compared with the well established methods of infrared spectroscopy and thin‐layer chromatography.


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