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Total assignment of the 1H- and 13C-NMR spectra of dinaphtho[1,2-b:1′,2′-d]thiophene through the concerted use of two-dimensional NMR techniques

✍ Scribed by Milton D. Johnston Jr.; Raymond N. Castle; Miguel Salazar; Diana K. Kruger; Gary E. Martin

Publisher
John Wiley and Sons
Year
1988
Tongue
English
Weight
731 KB
Volume
26
Category
Article
ISSN
0749-1581

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✦ Synopsis

The 'H-and I3C-NMR spectra of dinaphtho[l,2-b: l',Z-djthiophene (l), a sdfur-containing polynuclear heteroaromatic, have been totally assigned using a combination of two-dimensional NMR techniques. Techniques applied were standard proton-proton COSY, proton zeroquantum coherence (ZQCOSY, optimized to 7 Hz and to 1.75 Hz), proton double quantum coherence (DQCOSY, optimized to 7 Hz), broad-band decoupled (both dimensions) protonarbon chemical shift correlation, long-range proton-carbon chemical shift correlation, and proton-carbon heteronuclear relayed coherence transfer. A comparison of these methods on 1 showed the most useful information concerning connectivities to be obtained from the zeroquantum coherence and long-range heteronuclear correlation experiments. A detailed critique of each type of experiment is given in the context of applications to polynuclear aromatics.

KEY WORDS 2D NMR heteronuclear chemical shift correlation COSY double quantum coherence

zero quantum coherence relayed coherence transfer J-filtration long range heteronuclear shift correlation BIRD pulse

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