二维核磁共振谱原理.ppt

2D 核磁共振谱;;;;;;;COSY: Hypothetical Coupling;COSY: 1H-1H Coupling;;Coupling networks can be traced out, as shown in the figure below.? ? ;Table of COSY correlations;;;;What You See In a NOESY. . .;突出表现NOE效应的NOESY谱;;NOESY. . .;NOESY Spectrum of Codeine;Expansion of the upfield region: ;Table of NOEs: ( indicates the more upfield of geminal CH2 protons);;;2 D C-H相关谱（C-H COSY);2 D 远程C-H COSY;Heteronuclear Multiple Quantum Coherence (HMQC) and Heteronuclear Multiple Bond Coherence (HMBC): 2-D inverse H,C correlation techniques that allow for the determination of carbon (or other heteroatom) to hydrogen connectivity. ;HMQC (trans-ethyl 2-butenoate);HMQC – Heteronuclear Multiple-Quantum Coherence Experiment ;C(9)-H;HMQC?? (1-Bond CH Correlation) of Codeine;This is a 2D experiment used to correlate, or connect, 1H and 13C peaks for atoms separated by multiple bonds (usually 2 or 3).? The coordinates of each peak seen in the contour plot are the 1H and 13C chemical shifts.? This is extremely useful for making assignments and mapping out covalent structure. The information obtained is an extension of that obtained from an HMQC spectrum, but is more complicated to analyze.? Like HMQC, this is an inverse detection experiment, and is possible only on newer model spectrometers.? Acorn NMRs new JEOL Eclipse+ 400 is equipped to perform inverse experiments, and uses Z-gradients for improved spectral quality. The time required for an HMBC depends on the amount of material, but is much greater than for HMQC, and can take from an hour to overnight.;? Peaks occur at coordinates in the 2 dimensions corresponding to the chemical shifts of a carbon and protons separated by (usually) 2 or 3 bonds.? The experiment is optimized for couplings of ~8 Hz.? Smaller couplings are observed, but their intensities are reduced.? Compare to the spectrum obtained when the experiment is optimized for 4 Hz. The experiment is designed to suppress 1-bond correlations, but a few are observed in most s