Nuclear magnetic resonance spectroscopy HETCOR

Due to the great complexity of this class of molecules, nuclear magnetic resonance (NMR) and mass spectroscopy (MS) are the tools most widely used to identify cucurbitacins. Both one- and two-dimensional NMR techniques have been employed for the structural elucidation of new compounds 2D NMR, 1H-NMR, 13C-NMR, correlated spectroscopy (COSY), heteronuclear chemical shift correlation (HETCOR), attached proton test (APT), distortionless enhancement by polarization transfer (DEPT), and nuclear Overhauser effect spectroscopy (NOESY) are common techniques for determining the proton and carbon chemical shifts, constants, connectivity, stereochemistry, and chirality of these compounds [1,38,45-47]. 

We present a solid-state nuclear magnetic resonance (NMR) experiment that allows the observation of a high-resolution two-dimensional heteronuclear correlation (2D HETCOR) spectrum between aluminum and phosphorous in aluminophosphate molecular sieve VPI-5. The experiment uses multiple quantum magic angle spinning (MQMAS) spectroscopy to remove the second order quadrupolar broadening in Al nuclei. The magnetization is then transferred to spin-1/2 nuclei of P via cross polarization (CP) to produce for the first time isotropic resolution in both dimensions. 

Carbon peak assignments were not available in the earlier reports, and hence, a comprehensive study utilizing H, correlation spectroscopy (COSY), heteronuclear correlation (HETCOR), and heteronuclear multibond correlation (HMBC) nuclear magnetic resonance was undertaken. NMR CDCI3 (5 ppm vs. TMS (multiplicity H s coupling constant assignment)) 7.36 (d IH J5.4 Hz, H-2),... 

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