Aimed at Academic researchers, Industrialists and Postgraduates.
The following may be interested in buying the book:
The American Society of Pharmocognosy: http://www.phcog.org/
Association of Managers of Magnetic Resonance Labs: http://www.ammrl.org/
NMR Discussion Group: http://www.nmrdg.org.uk/
Society for Applied Spectroscopy http://www.s-a-s.org/home/
This text will appeal to those working in the structure elucidation of natural products as it
brings together a diverse but relevant selection of topics. It covers both methodology and
application to specific disciplines within natural product chemistry.
Die Inhaltsangabe kann sich auf eine andere Ausgabe dieses Titels beziehen.
Antony J. Williams graduated with a BSc and PhD in chemistry from the University of Liverpool and University of London respectively. He subsequently became a Post-doctoral Fellow at the National Research Council in Ottawa and then an NMR Facility Director at the University of Ottawa. He has also worked as an NMR Technology Leader at Eastman-Kodak Company in Rochester and held a number of positions, including Chief Science Officer, at ACD/Labs. In 2007, he established ChemZoo, Inc and became host of ChemSpider, one of the primary internet portals for chemistry. ChemSpider was acquired by the Royal Society of Chemistry (RSC) in 2009 and Dr Williams is currently Vice-President of Strategic Development at the RSC. He presently holds an adjunct position at UNC-Chapel Hill and has been a member of the ACS since 1996.
Gary E. Martin graduated with a BS in Pharmacy in 1972 from the University of Pittsburgh and a PhD in Pharmaceutical Sciences from the University of Kentucky in 1975, specializing in NMR spectroscopy. He was a Professor at the University of Houston from 1975 to 1989, assuming the position of Section Head responsible for US NMR spectroscopy at Burroughs Wellcome, Co. in Research Triangle Park, NC, eventually being promoted to the level of Principal Scientist. In 1996 he assumed a position at what was initially the Upjohn Company in Kalamazoo, MI and held several positions there through 2006 by which time he was a Senior Fellow at what was then Pfizer, Inc. In 2006 he assumed a position as a Distinguished Fellow at Schering-Plough responsible for the creation of the Rapid Structure Characterization Laboratory. He is presently a Distinguished Fellow at Merck Research Laboratories.
David Rovnyak earned his BS from the University of Richmond, and his PhD studying high resolution NMR of quadrupolar nuclei at MIT. He transitioned to solution phase biomolecular NMR in postdoctoral work at the Harvard Medical School before joining the Chemistry Department at Bucknell University, where he has been recognized with Bucknell's Excellence in Teaching Award. He currently serves as Assistant Editor of Concepts in Magnetic Resonance. His lab pursues interdisciplinary topics in biophysical research including bile acid aggregation, methods in protein NMR, nonuniform sampling and small molecule profiling.
The Ghanian plant Cryptolepis sanguinolenta is the source of a series of fascinating indoloquinoline alkaloids. The most unusual member of this alkaloid series was initially proposed to be a spiro nonacyclic structure, named cryptospirolepine, and was elucidated in 1993 based on the technologies available at that time. There were, however, several annoying attributes to the structure that bothered analysts for the ensuing 22 years. During the two decades that followed the initial work there have been enormous developments in NMR technology. Using new experimental approaches, specifically homodecoupled 1,1- and 1,n-HD-ADEQUATE NMR experiments developed in 2014, the structure of only a 700 µg sample of cryptospirolepine has been revised and is shown on the cover of this volume. The confluence of the NMR technological and methodological advances that allowed the revision of the structure of cryptospirolepine using a submilligram sample seems a fitting example for this book, which is dedicated to the NMR characterization of various classes of natural products.
Volume 2 considers data processing and algorithmic based analyses tailored to natural product structure elucidation and reviews the application of NMR to the analysis of a series of different natural product families including marine natural products, terpenes, steroids, alkaloids and carbohydrates. Volume 1 discusses contemporary NMR approaches including optimized and future hardware and experimental approaches to obtain both the highest quality and most appropriate spectral data for analysis. These books, bringing together acknowledged experts, uniquely focus on the combination of experimental approaches and modern hardware and software applied to the structure elucidation of natural products. The volumes will be an essential resource for NMR spectroscopists, natural product chemists and industrial researchers working on natural product analysis or the characterization of impurities and degradation products of pharmaceuticals that can be as scarce as natural product samples.
The Ghanian plant Cryptolepis sanguinolenta is the source of a series of fascinating indoloquinoline alkaloids. The most unusual member of this alkaloid series was initially proposed to be a spiro nonacyclic structure, named cryptospirolepine, and was elucidated in 1993 based on the technologies available at that time. There were, however, several annoying attributes to the structure that bothered analysts for the ensuing 22 years. During the two decades that followed the initial work there have been enormous developments in NMR technology. Using new experimental approaches, specifically homodecoupled 1,1- and 1,n-HD-ADEQUATE NMR experiments developed in 2014, the structure of only a 700 µg sample of cryptospirolepine has been revised and is shown on the cover of this volume. The confluence of the NMR technological and methodological advances that allowed the revision of the structure of cryptospirolepine using a submilligram sample seems a fitting example for this book, which is dedicated to the NMR characterization of various classes of natural products.
Volume 2 considers data processing and algorithmic based analyses tailored to natural product structure elucidation and reviews the application of NMR to the analysis of a series of different natural product families including marine natural products, terpenes, steroids, alkaloids and carbohydrates. Volume 1 discusses contemporary NMR approaches including optimized and future hardware and experimental approaches to obtain both the highest quality and most appropriate spectral data for analysis. These books, bringing together acknowledged experts, uniquely focus on the combination of experimental approaches and modern hardware and software applied to the structure elucidation of natural products. The volumes will be an essential resource for NMR spectroscopists, natural product chemists and industrial researchers working on natural product analysis or the characterization of impurities and degradation products of pharmaceuticals that can be as scarce as natural product samples.
Part 1,
Chapter 1 Application of the Nuclear Overhauser Effect to the Structural Elucidation of Natural Products R. R. Gil and A. Navarro-Vazquez, 3,
Chapter 2 Assigning Molecular Configuration by Nuclear Magnetic Resonance Kirk R. Gustafson, Susanna T. S. Chan and Yizhou Liu, 39,
Chapter 3 Nuclear Magnetic Resonance Experiments Applicable to the Elucidation and Characterization of Nitrogenous Natural Products: 1H-15N Heteronuclear Shift Correlation Methods Josep Sauri, Antony J. Williams and Gary E. Martin, 71,
Chapter 4 Application of Residual Dipolar Couplings to the Structural Analysis of Natural Products R. R. Gil and A. Navarro-Vazquez, 117,
Chapter 5 Applications of High-resolving Power, High-accuracy Mass Spectrometry for the Structural Elucidation of Natural Products Gary Kruppa and Wendy Zhong, 177,
Chapter 6 Current Pulse Sequence Developments in Small-molecule Nuclear Magnetic Resonance SpectroscopyTeodor Parella, 199,
Part 2,
Chapter 7 Terpenes: Mono-, Sesqui-, and Higher TerpenesWilliam F. Reynolds and Raul G. Enriquez, 253,
Chapter 8 Nuclear Magnetic Resonance of Steroids Martin Jaeger and Ruud L. E. G. Aspers, 275,
Chapter 9 Nuclear Magnetic Resonance Experiments Applicable to the Elucidation and Characterization of Alkaloid Structures Part I: Direct XH-13C Heteronuclear Shift Correlation and Establishing Contiguous Protonated Carbon Spin Systems Josep Sauri and Gary E. Martin, 315,
Chapter 10 Nuclear Magnetic Resonance Experiments Applicable to the Elucidation and Characterization of Alkaloid Structures Part II: Advanced Techniques for the Identification of Adjacent Carbons Using H2BC, 1,1 ADEQUATE, and Variants Josep Sauri and Gary E. Martin, 358,
Chapter 11 Nuclear Magnetic Resonance Case Studies in Marine Natural Products Angela A. Salim, Andrew M. Piggott and Robert J. Capon, 403,
Chapter 12 Nuclear Magnetic Resonance Case Studies in Microbial Natural Products Andrew M. Piggott, Angela A. Salim and Robert J. Capon, 440,
Chapter 13 Nuclear Magnetic Resonance in Saponin Structure Elucidation Antonio Jorge Ribeiro da Silva, Ricardo Moreira Borges and Vitor Soares, 486,
Chapter 14 Increasing the Adoption of Advanced Techniques for the Structure Elucidation of Natural Products Antony J. Williams, Gary E. Martin and David Rovnyak, 502,
References, 506,
Subject Index, 508,
Application of the Nuclear Overhauser Effect to the Structural Elucidation of Natural Products
R. R. GIL AND A. NAVARRO-VÁZQUEZ
The Historical Origin of the Term "Nuclear Overhauser Effect"
Albert W. Overhauser, while holding a postdoctoral position at the Department of Physics of the University of Illinois at Urbana (IL), theoretically proposed in 1953 that if the electron spin resonance of the conduction electrons in metals is saturated, the nuclei of the metal will be polarized to the same degree they would be if their gyromagnetic ratio were that of the electron spin. The nuclear spins would exhibit an enhanced polarization by a factor of [congruent to] 1000. Such a significant degree of polarization of the metal nuclei predicted by Overhauser was soon after experimentally demonstrated by Carver and Slichter in a sample of metallic lithium. This is the concept that led to a new field of study known as dynamic nuclear polarization (DNP), in which the electron spin polarization is transferred to nuclei in order to significantly improve their sensitivity. Although not the topic of this chapter, it is important to highlight that DNP is slowly becoming a very powerful tool in the structure analysis of molecules in high-resolution, solid-state nuclear magnetic resonance (NMR) spectroscopy, and led Professor Overhauser to receive the 1994 National Medal of Science.
Note, however, that the nuclear Overhauser effect (nOe), which is the nuclear-nuclear analog of the original electronic Overhauser effect, was first observed by I. Solomon in 1955. Following the studies on nuclear spin relaxation previously published by Bloembergen, Purcell, and Pound on a single-spin system, Solomon published a seminal article entitled "Relaxation Processes in a System of Two Spins". He experimentally observed that the longitudinal magnetization of a dipolar-coupled pair of "unlike" spins (different resonance frequencies) does not show simple exponential decay as in the case of a single-spin system. The experiments were done in an anhydrous sample of hydrofluoric acid. Upon saturation (steady-state Overhauser effect) or inversion (transient Overhauser effect) of the H resonance, a maximum increase of ~30% of the F signal was observed. The same effect was observed on the proton signal when the F resonance was excited in a similar way. Although not explicitly stated in Solomon's paper, this was the first reported experimental observation of the Overhauser effect between nuclei, and the experiment was later called the "nuclear Overhauser effect" and gave origin to the nOe or NOE acronym. This acronym can also be found in the literature standing for "nuclear Overhauser enhancement" due to the fact that the experiment produces enhancements of the NMR signals. We particularly prefer to use the term "effect". Solomon also set the theoretical basis of the NOE. He describes in his paper a set of modified Bloch equations that gives the correct equation of motion of the macroscopic magnetic moments for a system of two spins under the influence of dipole-dipole interaction. These equations are known today as the Solomon equations; the diagrams representing the Zeeman levels for a two-spin system are correspondingly known as the Solomon diagrams. Later in the chapter, we will come back to these equations and diagrams.
Intramolecular as well as intermolecular proton-proton NOEs were first reported by Reinhold Kaiser in 1963 and 1965, respectively. In the former article, Kaiser reported how the Overhauser effect can be used to determine the relative sign of J coupling constants, and to assign spectral lines to transitions between energy levels in trans-crotonaldehyde and m-dinitrobenzene. In the second article, Kaiser reported the intermolecular NOE in the liquid state between the protons of chloroform and cyclohexane.
Anet and Bourn introduced the first application of the NOE to the configurational and conformational analysis of small organic molecules in a seminal paper published in 1965. In this ground-breaking paper, they observed NOE enhancements when irradiating a sample of 3-methyl-but-2-enoic acid (1) and dimethylformamide (2), as well as in the half-cage acetate 3 (Figure 1.1). Prior to this article, the assignment of proton resonances in high-resolution spectra was performed on the basis of chemical shifts and J couplings. Shortly thereafter, Nakanishi applied intramolecular NOE analysis to the structural determination of the ginkgolides, a series of polyhydroxylated terpenoids. Irradiation of the ginkgolide C t-butyl group resulted in clear intensity enhancements that allowed the determination of the configuration of the related stereogenic centers (Figure 1.2). In the following year, the application of the NOE to taxane derivatives was also reported...
„Über diesen Titel“ kann sich auf eine andere Ausgabe dieses Titels beziehen.
Anbieter: PBShop.store US, Wood Dale, IL, USA
HRD. Zustand: New. New Book. Shipped from UK. Established seller since 2000. Artikel-Nr. CX-9781849733939
Anzahl: 15 verfügbar
Anbieter: PBShop.store UK, Fairford, GLOS, Vereinigtes Königreich
HRD. Zustand: New. New Book. Shipped from UK. Established seller since 2000. Artikel-Nr. CX-9781849733939
Anzahl: 15 verfügbar
Anbieter: Ria Christie Collections, Uxbridge, Vereinigtes Königreich
Zustand: New. In. Artikel-Nr. ria9781849733939_new
Anzahl: Mehr als 20 verfügbar
Anbieter: moluna, Greven, Deutschland
Gebunden. Zustand: New. The second volume in a two part set that discusses NMR analysis for the structure elucidation of natural products. It covers data acquisition tailored to natural product structure elucidation and applications to classes of natural products.Über. Artikel-Nr. 597106791
Anzahl: Mehr als 20 verfügbar
Anbieter: Revaluation Books, Exeter, Vereinigtes Königreich
Hardcover. Zustand: Brand New. 516 pages. 9.25x6.25x1.25 inches. In Stock. Artikel-Nr. x-1849733937
Anzahl: 2 verfügbar