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Structure Elucidation by Modern NMR: A Workbook by Prof. Dr. Helmut Duddeck, Dr. Wolfgang Dietrich, Prof. Dr.

By Prof. Dr. Helmut Duddeck, Dr. Wolfgang Dietrich, Prof. Dr. Gábor Tóth (auth.)

During the previous couple of years, regimen functions of NMR innovations were additional built. Spectrometers of the most recent new release provide new kinds of experiments, reminiscent of spinlock and inverse-detected tools. during this 3rd, revised and increased version, new method is brought and integrated into new workouts. furthermore, a brand new bankruptcy has been brought which demonstrates the totally certain interpretation of 2 common examples.

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It should be noted that the 2D spectra do not only offer a higher sensitivity and hence a shorter not carry an OH group), furthermore to C-4, C-23, and C-24, and then from H-24 to C-5. Further, we spectrometer time, but also a much higher content of information because the 13C,IH correlation is can reach H-25 from C-5. H-25 leads us to C-l, C-9, and C-lO. A connectivity from C-9 to H-26 is visible, and the determination of the individual IH obvious; the latter signal identifies two quaternary carbons (C-8 and C-14) as weil as C-7.

Irradiation of the acetyl methyl protons affords significant intensity enhancements for H-4 and for one ofthe aromatic protons, which apparently does not possess an ortho-positioned IH neighbor, since the signal is a narrow singlet and lacks a 7 - 9 Hz splitting. Owing to spatial proximity, this can only be H-6. So, it has to be concluded that the nitro group is attached to C-7. This simple experiment, requiring only a few minutes of spectrometer time, gives an answer to a question that could have been solved altematively only by establishing 13C, 13 C connectivities.

If it is possible to obtain a 1D broad-band decoupled 13c NMR spectrum of a given sampIe within a few minutes with a reasonable signal-to-noise ratio, a RETCOR spectrum can be obtained in less than one hour. Spectrometer time problems arise when the concentration is lower. In such cases the classical RETCOR experiment is inferior to variants using inverse detection mode [7], such as RSQC (Heteronuclear Single Quantum Correlation) and RMQC (Heteronuclear Multiple-Quantum Correlation). These experiments require some hardware modifications and specially designed probeheads.

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