Course: Advanced NMR Spectroscopy of Organic Compounds

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Course title Advanced NMR Spectroscopy of Organic Compounds
Course code UOCHT/CD169
Organizational form of instruction no contact
Level of course Doctoral
Year of study not specified
Semester Winter and summer
Number of ECTS credits 0
Language of instruction Czech
Status of course Compulsory-optional
Form of instruction Face-to-face
Work placements This is not an internship
Recommended optional programme components None
Lecturer(s)
  • Šimůnek Petr, doc. Ing. Ph.D.
Course content
Basic principles of NMR. A nucleus in magnetic field, macroscopic magnetization, Zeeman´s effect. Magnetogyric ratio. Population of spin states, nuclear resonance. Fourier-transform NMR, FID. Single pulse experiment. Pulse angle. Relaxation: processes and mechanisms. Relaxation agents, effect of paramagnetic materials on relaxation. Quadrupole nuclei. Signal-to-noise ratio. NMR spectrum. Chemical shift, its definition and meaning. Integral intensity. Shielding and its mechanisms. Diamagnetic and paramagnetic shift. Anisotropic effects. NMR and molecular symmetry. Corelation between chemical shift and structure. Spin-spin couplings, their origin. Spin-spin coupling constant. First-order systems, conditions for their appearance and how to affect them. Multiplicity rule, intensity rule. Magnetic equivalence of nuclei. Spectra of higher-order systems. Correlation between coupling constant and structure. Heteronuclear and homonuclear decoupling, broadband and selective decoupling. Gated and inverse-gated decoupling. Importance of decoupling and its use. Advanced 1D experiments. APT. Polarization and its transfer. Polarisation-transfer techniques. DEPT. Selective excitation. Energy of pulse, soft and hard pulses. Selective COSY, TOCSY, HMQC, their importance and use. 2D NMR spectroscopy. Basic principles. Homonuclear correlations. H,H-COSY ,TOCSY, 2D-INADEQUATE, use and interpretation. Heteronuclear correlations. Inverse detection. Single-bond correlations, HMQC, HSQC, use, interpretation. Long-range correlations, HMBC, use, interpretation. Hybrid experiments: HSQC-DEPT, HMQC-TOCSY, use, interpretation.. NOE spectroscopy. Dipolar interactions. Nuclear Overhauser Effect, origin, effect on spectrum. NOE difference spectrum, use and interpretation. 1D a 2D NOESY, use and interpretation. 1D and 2D ROESY, use and interpretation. Dynamic NMR spectroscopy. Chemical exchange. Spectroscopic time-scales. Effect of dynamic processes on NMR spectra, effect of temperature and solvent. Study of dynamic processes by means of NMR, hindered rotations, conformational changes, fast reversible processes, inter and intramolecular hydrogen bonds. Quantitative evaluation of slow and fast processes. EXSY.

Learning activities and teaching methods
Dialogic (discussion, interview, brainstorming), Work with text (with textbook, with book)
Learning outcomes
The aim of the subject is to deepen and extend knowledge on NMR spectroscopy gained during MSc. study.
Ability of autonomous study, information survey, precision, conscientiousness.
Prerequisites
Knowledge on NMR spectroscopy at the MSc. level.

Assessment methods and criteria
Oral examination

For the graduation from the subject it is necessary to successfully pass through the oral exam. It comprises both consideration of the ability of the student to interpret various kinds of spectra including the suggestion how to solve particular problems and the extent of understanding the theoretical background of individual techniques.
Recommended literature
  • Claridge T. D. W. High-Reolution NMR Techniques in Organic Chemistry. Amsterdam, 1999. ISBN 0-08-042798-7.
  • Croasmun W. R., Carlson R. M. K. Two-Dimensional NMR Spectroscopy, Applications for Chemists and Bichemists. Weinheim, 1994. ISBN 1-56081-664-3.
  • Derome A. E. Modern NMR Techniques for Chemistry Research. Oxford, 1987. ISBN 0-08-032514-9.
  • Jacobsen N.E. NMR Spectroscopy Explained. New Jersey, 2007. ISBN 978-0-471-73096-5.
  • Sanders J.K.M., Hunter B. K. Modern NMR Spectroscopy, A Guide for Chemists. Oxford, 1993. ISBN 0-19-855567.


Study plans that include the course
Faculty Study plan (Version) Category of Branch/Specialization Recommended year of study Recommended semester