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Ultra-high resolution band-selective HSQC for nanomole-scale identification of chlorine-substituted 13 C in natural products drug discovery.
Wang, Xiao; Duggan, Brendan M; Molinski, Tadeusz F.
Afiliación
  • Wang X; Department of Chemistry and Biochemistry, University of California San Diego, 9500 Gilman Dr. MC-0358, La Jolla, CA, USA.
  • Duggan BM; Skaggs School of Pharmacy and Pharmaceutical Sciences, University of California San Diego, 9500 Gilman Dr. MC-0358, La Jolla, CA, USA.
  • Molinski TF; Department of Chemistry and Biochemistry, University of California San Diego, 9500 Gilman Dr. MC-0358, La Jolla, CA, USA.
Magn Reson Chem ; 55(4): 263-268, 2017 Apr.
Article en En | MEDLINE | ID: mdl-26951950
Ultra-high resolution band-selective HSQC (bsHSQC) has been employed for detection of 35 Cl-37 Cl isotope shifted 13 C NMR signals for assignment of regioisomerism in bromo-chloro natural products. Optimum pulse sequence and instrumental parameters for maximization of detection of the isotope shifts were explored. The chlorine isotope shifts (Δδ) were detected within crosspeaks and were shown to vary with hybridization of 13 C, substitution of 13 C, presence of ß-chloro substituents, and their relative configuration. Deconvolution of Cl-substituted CH bsHSQC crosspeaks may provide other useful information, including a potentially MS-independent method for quantitating 37 Cl/35 C isotopic fractionation during the biosynthesis of halogenated natural products. Copyright © 2016 John Wiley & Sons, Ltd.
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Texto completo: 1 Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Productos Biológicos / Espectroscopía de Resonancia Magnética / Cloro Tipo de estudio: Diagnostic_studies Límite: Humans Idioma: En Revista: Magn Reson Chem Asunto de la revista: QUIMICA Año: 2017 Tipo del documento: Article País de afiliación: Estados Unidos Pais de publicación: Reino Unido

Texto completo: 1 Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Productos Biológicos / Espectroscopía de Resonancia Magnética / Cloro Tipo de estudio: Diagnostic_studies Límite: Humans Idioma: En Revista: Magn Reson Chem Asunto de la revista: QUIMICA Año: 2017 Tipo del documento: Article País de afiliación: Estados Unidos Pais de publicación: Reino Unido