NMR: FROM SPECTRA TO STRUCTURES
INTRODUCTION PART 1: NMR EXPERIMENTS 1D EXPERIMENTS 1H, D (2H): NATURAL ABUNDANCE, SENSITIVITY 1 1 PROTON NMR SPECTRUM OF THE MODEL COMPOUND 1 FIELD DEPENDENCE OF THE SPECTRUM OF 1 FID MANIPULATION: FT, EM, SINE BELL (CH2 SIGNAL OF 1) THE PROTON SPECTRUM OF 1 IN D2O OR H2O/D2O MIXTURES INTEGRATION: RELAXATION, T1, 90°-PULSE, ERNST ANGLE THE NOE: THROUGH-SPACE INTERACTIONS BETWEEN PROTONS 1 1 6 1 NOE DIFFERENCE SPECTROSCOPY 1 1 6 2 SELECTIVE 1D NOE EXPERIMENT (1D-NOESY) AND SELECTIVE 1D TOCSY EXPERIMENT 13C 1 2 NATURAL ABUNDANCE 13C SPECTRUM OF COMPOUND 1 COUPLED SPECTRUM (GATED DECOUPLING) QUANTITATIVE 13C SPECTRUM (INVERSE GATED DECOUPLING) DECOUPLED SPECTRUM: PROTON DECOUPLING, PROTON AND PHOSPHORUS DECOUPLING APT, DEPT, INEPT THE INADEQUATE EXPERIMENT 31P 1 3 NATURAL ABUNDANCE 31P SPECTRUM OF COMPOUND 6 PROTON-DECOUPLED AND PROTON-COUPLED SPECTRA COUPLED SPECTRUM (P–P COUPLING) 2D EXPERIMENTS GENERAL PRINCIPLES, INVERSE TECHNIQUES, GRADIENTS H,H COSY 2D NOE P,H COSY: WITH VARYING MIXING TIMES FOR THE COUPLING C,H DIRECT CORRELATION C,H LONG RANGE CORRELATION P,C CORRELATION P,P CORRELATION QUADRUPOLAR NUCLEUS EXPERIMENTS GENERAL PRINCIPLES: QUADRUPOLE MOMENT, RELAXATION, LINEWIDTH 17O 3 2 17O SPECTRUM OF 7: CHEMICAL SHIFT (REFERENCE), COUPLING WITH P P–O CORRELATION HPLC-NMR COUPLING GENERAL PRINCIPLES, NMR AS A HIGHLY SENSITIVE ANALYTICAL TOOL (?G TO NG AMOUNTS) EXAMPLE: SEPARATION OF 4 AND 5, TWO ACETALS OF FORMYLPHOSPHONIC ESTER CHROMATOGRAM ON-FLOW DIAGRAM (CHEMICAL SHIFT VS TIME) STOPPED FLOW EXPERIMENTS OTHER SPIN-½ NUCLEI 15N 19F 29SI 77SE 113CD 117SN, 119SN 195PT 207PB SOLID STATE NMR GENERAL PRINCIPLES SOLID STATE 1H NMR SOLID STATE 13C NMR SOLID-STATE 31P NMR SOLID-STATE 29SI NMR APPENDIX: REFERENCE LIST PART 2: WORKED EXAMPLE AND PROBLEMS SECTION 1 SOLVING THE STRUCTURES OF ORGANIC MOLECULES ELEMENTAL ANALYSIS MASS SPECTROMETRY WORKED EXAMPLE H,H CORRELATION C,H CORRELATION PROBLEMS SECTION 2