Pharmaceutical Sciences 491
Special Topics in NMR Spectroscopy
Fall 2005
Thomas
C. Stringfellow, Instructor
Office:
(608) 262–4237
NMR Lab:
(608) 262–1589
E-mail:
tcstringfellow@pharmacy.wisc.edu
| Course Syllabus | Course syllabus, including topic outline, goals, grading, expectations, guidelines, etc. |
| Companion Text | Text by T. C. Stringfellow provides background on quantum mechanics, density matrix theory and spin relaxation theory as supplemental information for those interested. |
| Questionnaire | A brief questionnaire to gather background information about the students' training and experience with NMR and other related topics. |
| Lecture Notes | Notes, outlines, etc. from class lectures. |
| Problem Sets | Optional problem sets (will not be graded) are designed to provide practice and develop insight. |
| Homework | Homework assignments, primarily laboratory based. |
| Exams and Quizzes | Lecture and laboratory exams and quizzes. |
| Supporting Materials | Additional resources to support or supplement lectures and laboratory exercises. |
| The Basics of MRI | This is an interesting and relevant electronic textbook, with many interactive features, describing magnetic resonance imaging (MRI). Chapters 2–5 cover background material that should be largely familiar to students at this point in our course; chapters 6–14 focus on various aspects of imaging, including several clinical images. This link is included here for the interested students. |
Lecture Notes and Outlines
| Front Matter | Lecture notes "book" cover, table of contents, etc. |
| Lecture No. 0 | Course introduction and preliminary comments |
| Lecture No. 1 | Historical perspective of NMR |
| Lecture No. 2 | Introduction to NMR theory: Classical and Quantum descriptions (light version); the strong-to-weak coupling continuum |
| Lecture No. 3 | Spectral information content; Case study: Neamine at pH = 1.5 |
| Lecture No. 4 | Introduction to pulsed, FT NMR |
| Lecture No. 5 | Sensitivity and other practical issues |
| Lecture No. 6 | The second dimension |
| Lecture No. 7 | Homonuclear correlation experiments |
| Lecture No. 8 | Heteronuclear correlation experiments |
| Lecture No. 9 | Nuclear spin relaxation |
| Lecture No. 10 | The nuclear Overhauser effect (NOE) |
| Lecture No. 11 | Dynamic NMR |
| Lecture No. 12 | Measuring translational self-diffusion via NMR |
Problem Sets
| Problem Set No. 1 | Nuclear spin energy contributions and thermal energy, populations, chemical shielding dispersion |
| Problem Set No. 2 | Energy-level diagrams for simple spin systems |
| Problem Set No. 3 | The upfield, downfield paradox |
| PS 3 Solution | Solution guide to Problem Set No. 3 |
| Problem Set No. 4 | Vector picture of NMR in the laboratory and rotating frames, including the effects of pulses |
| Problem Set No. 5 | Digital resolution and the corresponding acquisition parameters |
| PS 5 Solutions | Solution guide to Problem Set No. 5 |
| Problem Set No. 6 | Practical sensitivity issues related to instrumentation, sample concentration, experiment time, etc. |
| PS 6 Solutions | Solution guide to Problem Set No. 6 |
| Problem Set No. 7 | Exercises 1–13 in Chapter 5 of Structure Elucidation by Modern NMR: A Workbook |
Homework Assignments
| Homework No. 0 | NMR stick spectra of structural isomers (optional exercise) |
| Homework No. 1 | ACD Labs ChemSketch, HNMR and CNMR Predictors |
| Homework No. 2 | Introduction to computers and Varian's VNMR software for basic data processing |
| Homework No. 3 | Lab safety revisited; NMR acquisition basics: 1D 1H data acquisition and analysis |
| Homework No. 4 | 1D 13C data: routine versus DEPT spectra |
| Homework No. 5 | Homonuclear 2D NMR: the basic 1H–1H COSY experiment |
| Homework No. 6 | The DQCOSY and TOCSY experiments |
| Homework No. 7 | One-bond heteronuclear correlations: the HSQC and HMQC experiments |
| Homework No. 8 | Multiple-bond heteronuclear correlations: the HMBC experiment |
| Homework No. 9 | Spatial correlations: the NOESY and ROESY experiments |
| Homework No. 10 | Measuring translational diffusion, kinetics and spin relaxation |
Exams and Quizzes
| Quiz No. 1 | Tuesday, 27 September 2005 |
| Lecture Exam No. 1 | First lecture exam: Tuesday, 18 October 2005 |
| Lab Exam No. 1 | First laboratory exam: Wednesday, 19 October 2005 |
| Quiz No. 2 | Tuesday, yy October 2005 |
| Quiz No. 3 | Tuesday, zz November 2005 |
| Lecture Exam No. 2 | Second lecture exam: Tuesday, 13 December 2005 |
| Lab Exam No. 2 | To be announced |
Supporting Materials
| Org. Lett. 5, 605–608, 2003. | How Do Ring Currents Affect 1H NMR Chemical Shifts?, C.S. Wannere and P.v.R. Schleyer. |
| Cavanagh, Chap. 6 | Sections 6.2.1 through 6.2.1.5 from Protein NMR Spectroscopy: Principles and Practice, by Cavanagh et al., Academic Press, 1996. This material discusses basic COSY experiments and the measurement of J couplings. |
| Magn. Reson. Chem. 35, 505–519, 1997. | Investigation of the Advantages and Limitations of Forward Linear Prediction for Processing 2D Data Sets, W.F. Reynolds, M. Yu, R.G. Enriques and I. Leon |
| Magn. Reson. Chem. 39, 531–538, 2001. | Gradient-selected versus Phase-cycled HMBC and HSQC: Pros and Cons, W.F. Reynolds and R.G. Enriques |
| J. Nat. Prod. 65, 221–224, 2002. | Choosing the Best Pulse Sequences, Acquisition Parameters, Postacquisition Processing Strategies, and Probes for Natural Product Structure Elucidation by NMR Spectroscopy, W.F. Reynolds and R.G. Enriques |
NMR Facility Home || Analytical Instrumentation Center || School of Pharmacy || UW–Madison Home || MyUW || UW Search