Structure nuclear magnetic resonance spectroscopy

Present day techniques for structure determination in carbohydrate chemistry are sub stantially the same as those for any other type of compound The full range of modern instrumental methods including mass spectrometry and infrared and nuclear magnetic resonance spectroscopy is brought to bear on the problem If the unknown substance is crystalline X ray diffraction can provide precise structural information that m the best cases IS equivalent to taking a three dimensional photograph of the molecule... 

GM Clore, MA Robien, AM Gronenborn. Exploring the limits of precision and accuracy of protein structures determined by nuclear magnetic resonance spectroscopy. J Mol Biol 231 82-102, 1993. 

Wiithrich, K. Protein structure determination in solution by nuclear magnetic resonance spectroscopy. Science 243 45-50, 1989. 

An X-ray crystallographic study of 2-hydroxy-4,6-dimethylpyrimi-dine led to no conclusions regarding its structure. Because of the rapid exchange of the NH protons of pyrimidin-2-one both in dimethyl sulfoxide and in water, nuclear magnetic resonance spectroscopy does not afford positive evidence for either the oxo or the hydroxy formulation. The statement that 4,6-dimethylpyrimidin-2-one had been isolated in two modifications, 94 and 95, was soon disproved. ... 

It is interesting to note that the acyclic analog, nitroguanidine, exists in the symmetrical form 288 rather than as 289. Structure 288 has been established by ultraviolet and proton nuclear magnetic resonance spectroscopy. X-ray crystallography, dipole moments, and ipK measurements (see reference 367 and references therein). 

Other methods of identification include the customary preparation of derivatives, comparisons with authentic substances whenever possible, and periodate oxidation. Lately, the application of nuclear magnetic resonance spectroscopy has provided an elegant approach to the elucidation of structures and stereochemistry of various deoxy sugars (18). Microcell techniques can provide a spectrum on 5-6 mg. of sample. The practicing chemist is frequently confronted with the problem of having on hand a few milligrams of a product whose structure is unknown. It is especially in such instances that a full appreciation of the functions of mass spectrometry can be developed. 

Determining the structure of an organic compound was a difficult and time-consuming process in the 19th and early 20th centuries, but powerful techniques are now available that greatly simplify the problem. In this and the next chapter, we ll look at four such techniques—mass spectrometry (MS), infrared (IR) spectroscopy, ultraviolet spectroscopy (UV), and nuclear magnetic resonance spectroscopy (NMR)—and we U see the kind of information that can be obtained from each. 

We saw in Chapter 12 that mass spectrometry gives a molecule s formula and infrared spectroscopy identifies a molecule s functional groups. Nuclear magnetic resonance spectroscopy does not replace either of these techniques rather, it complements them by "mapping" a molecule s carbon-hydrogen framework. Taken together, mass spectrometry, JR, and NMR make it possible to determine the structures of even very complex molecules. 

CHAPTER 13 Structure Determination Nuclear Magnetic Resonance Spectroscopy... 

Mass spectrometry, infrared spectroscopy, and nuclear magnetic resonance spectroscopy are techniques of structure determination applicable to all organic molecules. In addition to these three generally useful methods, there s a fourth—ultraviolet (UV) spectroscopy—that is applicable only to conjugated systems. UV is less commonly used than the other three spectroscopic techniques because of the specialized information it gives, so we ll mention it only briefly. 

Woolley RG (1982) Natural Optical Acitivity and the Molecular Hypothesis. 52 1-35 Wiithrich K (1970) Structural Studies of Hemes and Hemoproteins by Nuclear Magnetic Resonance Spectroscopy. 8 53-121... 

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