Heteronuclear multiple-bond correlations proton detected

Figure 11 Proton detected Heteronuclear Multiple Bond Correlation (HMBC) experiment [11]...

For smaller quantities of compounds more sensitive inverse detected techniques are available, such as HMQC ( IH-I C one bond correlation via heteronuclear multiple quantum coherence, analogous to HETCOR) and HMBC (proton detected heteronuclear multiple bond correlation spectroscopy) (15). The last provide, in addition to the intraresidue multiple bond correlations, interresidue correlations between the anomeric carbon and the aglycone protons.We follow this general strategy for the structural determination of tri terpenoid saponins of Bupleurum fruticosum (16) andArdisia japonica (9). 

Two-dimensional C//correlations such as C//COSY or HC HMQC and HSQC provide the Jqh connectivities, and thereby apply only to those C atoms which are linked to H and not to non-protonated C atoms. Modifications of these techniques, also applicable to quaternary C atoms, are those which are adjusted to the smaller Jqh and Jqh couplings (2-25 Hz, Tables 2.8 and 2.9) Experiments that probe these couplings include the CH COLOC (correlation via long range couplings) with carbon-13 detection (Fig. 2.16) and HC HMBC (heteronuclear multiple bond coherence) with the much more sensitive proton detection (Fig. 2.17)... 

The heteronuclear multiple-quantum correlation (HMQC) experiment is one of the two commonly employed proton-detected single-bond correlation experiments. Although this was suggested many years ago [1,2], the experiment lacked widespread use until a scheme was presented [3] that was able to overcome the technical difficulties associated with proton observation described above. Since then, and particularly since the advent of PFGs, the technique has come to dominate organic NMR spectroscopy. 

For the HMQC described above, we wanted an experiment that eliminated long-range (i.e., two and three bond) proton-carbon couplings while preserving the directly attached (i.e., one-bond) couplings, which we correlated in a 2-D experiment. The HMBC (Heteronuclear Multiple Bond Coherence) experiment, on the other hand, which is also proton detected, capitalizes... 

A H(detected)- C shift correlation spectrum (common acronym HMQC, for heteronuclear multiple quantum coherence, but sometimes also called COSY) is a rapid way to assign peaks from protonated carbons, once the hydrogen peaks are identified. With changes in pulse timings, this can also become the HMBC (heteronuclear multiple bond connectivity) experiment, where the correlations are made via the... 

Proton-detected two-dimensional (2D) NMR experiments, essentially based on two difierent pulse schemes referred to as heteronuclear single-quantum correlation (HSQC) [1] and heteronuclear multiple-quantum correlation (HMQC) [2], have been key NMR tools during many years for chemists and biochemists to provide valuable structural information on H- C (and H- N) chemical bonds in a molecule. Nowadays, these experiments are usually performed in a complete automation mode in both data acquisition and processing steps, practically without any need for direct user intervention. The resulting 2D maps are very simple to analyze and to interpret, even for non-experienced NMR users, typically displaying well-dispersed cross-peaks that correlate (direct F2 dimension) and (indi-... 

HC HMQC (heteronuclear multiple quantum coherence) and HC HSQC (heteronuclear single quantum coherence) are the acronyms of the pulse sequences used for inverse carbon-proton shift correlations. These sensitive inverse experiments detect one-bond carbon-proton connectivities within some minutes instead of some hours as required for CH COSY as demonstrated by an HC HSQC experiment with a-pinene in Fig. 2.15. 

HMQC Heteronuclear multiple quantum coherence, e.g. inverse CH correlation via one-bond carbon proton-coupling, same format and information as described for ( C detected) CH COSY but much more sensitive (therefore less time-consuming) because of H detection... 

---