Determination of ligand environment in solution in Gif type systems using quantitative 13C-NMR spectroscopy

New Journal of Chemistry

Volumn 20, Issue 1, 1996, Pages 121-124

  Barton, Derek H R ^a   Hu, Bin ^a   Rojas Wahl, Roy U ^a   Taylor, Dennis K ^a  

^a TEXAS A AND M UNIVERSITY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 0000661162     PISSN: 11440546     EISSN: None     Source Type: Journal    
DOI: None     Document Type: Article

References (27)

1. The Activation of Dioxygen and Homogeneous Catalytic Oxidation, Barton D. H. R., Martell A. E., Sawyer D. T., Eds., Plenum, New York, 1993.
2. (a) Shilov A. E., Activation of Saturated Hydrocarbons by Transition Metal Complexes, Reidel, Dordrecht, 1984.
3. (b) Activation and Functionalization of Alkanes, Hill C. L., Ed., Wiley, New York, Chichester, 1989.
4. (a) Barton D. H. R., Doller D., Acc. Chem. Res., 1992, 25, 504 and references cited therein.
5. (b) For industrial perspectives see: Schuchardt U., Carvalho W. A., Spinacé E. V., Synlett, 1993, 713.
6. For a comprehensive overview see: Balavoine G., Barton D. H. R., Geletii Y. V., Hill D. R., p. 225 in ref. [1], and references therein.
7. Barton D. H. R., Bévière S. D., Chavasiri W., Csuhai E., Doller D., Liu W. G., J. Am. Chem. Soc., 1992, 114, 2147.
8. Barton D. H. R., Csuhai E., Doller D., Balavoine G., J. Chem. Soc., Chem. Commun., 1990, 1787.
9. Barton D. H. R., Halley F., Ozbalik N., Young E., Balavoine G., Gref A., Boivin J., New J. Chem., 1989, 13, 177.
10. (a) Sheu C., Richert S. A., Cofré P., Ross Jr. B., Sobkowiak A., Sawyer D. T., Kanofsky J. R., J. Am. Chem. Soc., 1990, 112, 1936.
11. (b) Sheu C., Sobkowiak A., Jeon S., Sawyer D. T., J. Am. Chem. Soc., 1990, 112, 879.
12. (c) About-Jaudet E., Barton D. H. R., Csuhai E., Ozbalik N., Tetrahedron Lett., 1990, 31, 1657.
13. Barton D. H. R., Bévière S. D., Chavasiri W., Doller D., Liu W. G., Reibenspies J. H., New J. Chem., 1992, 16, 1019.
14. For a system using ferrous iron and two equivalents of picolinic acid see: Balavoine G., Barton D. H. R., Boivin J., Gref A., Tetrahedron Lett., 1990, 31, 659.
15. For short and comprehensive overviews see for example: (a) Friebolin H., Ein- und zweidimensionale NMR-Spektroskopie-eine Einführung, VCH, Weinheim, 1988, p. 28.
16. 13C NMR Spectroscopy - A Working Manual with Exercises, MMI Press Polymer Monograph Series, Vol. 3, Harwood, 1984, chap. 9 (6).
17. (c) Kasler F., Quantitative Analysis by NMR Spectroscopy, Academic, New York, 1973, chap. 14.
18. (d) Levy G. C., Lichter R. L., Nelson G. L., Carbon-13 Nuclear Magnetic Resonance Spectroscopy, Wiley, New York, 1980.
19. For more detailed overviews and further references see for example: (e) Mareci T. H., Scott K. N., Anal. Chem., 1977, 49, 2130.
20. (f) Shoolery J. N., Prog. Nucl. Magn. Res. Spectrosc., 1977, 11, 79.
21. (g) Mooney J. R. Field L. D., Analytical NMR, Sternhell S., Ed., Wiley, Chichester, New York, 1989, p. 41.
22. Hyperfine interaction, more efficient than dipole-dipole relaxation.
23. Several delays up to 3 s were applied. The quantification results were not affected by these precautions.
24. Hyperfine interaction between electron spin and the attached carbon nuclei leads to exceptionally fast relaxation and therefore no signals can be detected.
25. No significant line broadening is observed.
26. For limitations using paramagnetic relaxation reagents see for example: Levy G. C., Edlund U., J. Am. Chem. Soc., 1975, 97, 4482 and references therein.
27. As we often followed the course of a reaction, we needed a large spectral window. Smaller spectral windows gave similar quantification results. Thus the quantification results are not impaired by this large spectral window.