GET-SERF, a new gradient encoded SERF experiment for the trivial edition of 1H-19F couplings

被引:23
作者
Di Pietro, Maria Enrica [1 ,2 ]
Aroulanda, Christie [1 ]
Merlet, Denis [1 ]
机构
[1] Univ Paris 11, UMR 8182, ICMMO, Equipe RMN Milieu Oriente, Orsay, France
[2] Univ Calabria, Dipartimento Chim, LXNMRSCAn, Arcavacata Di Rende, CS, Italy
关键词
NMR spectroscopy; Fluorinated compounds; Couplings extraction; Spatial encoding; SERF experiment; MEDICINAL CHEMISTRY; DIPOLAR COUPLINGS; NMR-SPECTROSCOPY; H-1-NMR SPECTRA; FLUORINE; CONSTANTS; ENANTIOMERS; DEPENDENCE; PHARMACEUTICALS; HETERONUCLEAR;
D O I
10.1016/j.jmr.2013.06.011
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A new spatially encoded heteronuclear H-1-F-19 selective refocusing NMR experiment (GET-SERF) is proposed. This sequence allows editing in one single 2D experiment all couplings between a selected fluorine site and all the proton nuclei of the molecule. Its efficiency is illustrated in the case of diflunisal, a difluorinated anti-inflammatory drug, in isotropic and anisotropic media. (C) 2013 Elsevier Inc. All rights reserved.
引用
收藏
页码:101 / 105
页数:5
相关论文
共 49 条
[1]   Through space spin-spin coupling 19F-1H as the base for comparative analysis of conformational equilibrium in fluorine-substituted aryl vinyl selenides and sulfides [J].
Afonin, A. V. .
RUSSIAN JOURNAL OF ORGANIC CHEMISTRY, 2010, 46 (09) :1313-1316
[2]   Decoupling Two-Dimensional NMR Spectroscopy in Both Dimensions: Pure Shift NOESY and COSY [J].
Aguilar, Juan A. ;
Colbourne, Adam A. ;
Cassani, Julia ;
Nilsson, Mathias ;
Morris, Gareth A. .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2012, 51 (26) :6460-6463
[3]   Pure Shift 1H NMR: A Resolution of the Resolution Problem? [J].
Aguilar, Juan A. ;
Faulkner, Stephen ;
Nilsson, Mathias ;
Morris, Gareth A. .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2010, 49 (23) :3901-3903
[4]   Enantiomeric discrimination by double quantum excited selective refocusing (DQ-SERF) experiment [J].
Baishya, Bikash ;
Prabhu, Uday Ramesh ;
Suryaprakash, N. .
JOURNAL OF PHYSICAL CHEMISTRY B, 2007, 111 (43) :12403-12410
[5]   NUCLEAR-SPIN SPIN COUPLING VIA NONBONDED INTERACTIONS .4. IMPORTANCE OF BRIDGEHEAD INTERACTIONS ON VICINAL C-13-F-19 AND LONG-RANGE H-1-F-19 COUPLING-CONSTANTS IN 1-FLUOROBICYCLOALKANES [J].
BARFIELD, M ;
DELLA, EW ;
PIGOU, PE ;
WALTER, SR .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1982, 104 (13) :3549-3552
[6]   Recent advances (1995-2005) in fluorinated pharmaceuticals based on natural products [J].
Begue, Jean-Pierre ;
Bonnet-Delpon, Daniele .
JOURNAL OF FLUORINE CHEMISTRY, 2006, 127 (08) :992-1012
[7]   Improvements to selective refocusing phased (SERFph) experiments [J].
Beguin, L. ;
Giraud, N. ;
Ouvrard, J. M. ;
Courtieu, J. ;
Merlet, D. .
JOURNAL OF MAGNETIC RESONANCE, 2009, 199 (01) :41-47
[8]   Simplification of the 1H NMR spectra of enantiomers dissolved in chiral liquid crystals, combining variable angle sample spinning and selective refocusing experiments [J].
Beguin, Laetitia ;
Courtieu, Jacques ;
Ziani, Latifa ;
Merlet, Denis .
MAGNETIC RESONANCE IN CHEMISTRY, 2006, 44 (12) :1096-1101
[9]   GRAPHICAL INTERACTIVE STRATEGY FOR THE ANALYSIS OF NMR-SPECTRA IN LIQUID-CRYSTALLINE PHASES [J].
CELEBRE, G ;
DELUCA, G ;
LONGERI, M ;
SICILIA, E .
JOURNAL OF CHEMICAL INFORMATION AND COMPUTER SCIENCES, 1994, 34 (03) :539-545
[10]   Use of F-19 NMR to probe protein structure and conformational changes [J].
Danielson, MA ;
Falke, JJ .
ANNUAL REVIEW OF BIOPHYSICS AND BIOMOLECULAR STRUCTURE, 1996, 25 :163-195