Measurement of 1H NMR relaxation times in complex organic chemical systems: application of PSYCHE

被引：13
作者：
Kakita, Veera Mohana Rao [1 ]
Shukla, Vaibhav Kumar [1 ]
Bopardikar, Mandar [2 ]
Bhattacharya, Tannistha [3 ]
Hosur, Ramakrishna V. [1 ,2 ]
机构：
[1] Univ Mumbai, UM DAE Ctr Excellence Basic Sci, Kalina Campus, Mumbai 400098, Maharashtra, India
[2] TIFR, Dept Chem Sci, 1 Homi Bhabha Rd, Mumbai 400005, Maharashtra, India
[3] Natl Inst Technol, Dept Chem, Jamshedpur 831014, Bihar, India
来源：
RSC ADVANCES | 2016年 / 6卷 / 102期
关键词：
N-HETEROCYCLIC CARBENE; H BOND ACTIVATION; EFFECTIVE CORE POTENTIALS; OLEFIN METATHESIS CATALYSTS; PURE SHIFT NMR; C-H; MOLECULAR CALCULATIONS; COUPLING-CONSTANTS; METHYL GROUP; ALCOHOL DEHYDROGENATION;
D O I：
10.1039/c6ra20047h
中图分类号：
O6 [化学];
学科分类号：
0703 ;
摘要：
Relaxation times provide a wealth of information on intramolecular dynamics and intermolecular interactions. However, in complex molecular systems with extensive peak overlaps in NMR spectra, relaxation time measurements are severely hampered due to difficulties in quantitation of peak intensities for individual protons. Here, we incorporate PSYCHE homodecoupling in inversion recovery and CPMG NMR experiments to significantly enhance spectral resolution, thereby enabling unambiguous measurement of relaxation times, T-1 and T-2, in two complex systems. This includes a specific application to study drug-protein interactions.
引用
收藏
页码：100098 / 100102
页数：5
相关论文
共 76 条
[1]   Ruthenium carbene complexes with imidazolin-2-ylidene ligands allow the formation of tetrasubstituted cycloalkenes by RCM [J].
Ackermann, L ;
Fürstner, A ;
Weskamp, T ;
Kohl, FJ ;
Herrmann, WA .
TETRAHEDRON LETTERS, 1999, 40 (26) :4787-4790
[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]   Simple Proton Spectra from Complex Spin Systems: Pure Shift NMR Spectroscopy Using BIRD [J].
Aguilar, Juan A. ;
Nilsson, Mathias ;
Morris, Gareth A. .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2011, 50 (41) :9716-9717
[4]  
[Anonymous], 1995, ALL ALBUMIN
[5]   Looking for stable carbenes: The difficulty in starting anew [J].
Arduengo, AJ .
ACCOUNTS OF CHEMICAL RESEARCH, 1999, 32 (11) :913-921
[6]   EXPERIMENTAL ASPECTS OF CHIRP NMR-SPECTROSCOPY [J].
BOHLEN, JM ;
BODENHAUSEN, G .
JOURNAL OF MAGNETIC RESONANCE SERIES A, 1993, 102 (03) :293-301
[7]   Reversible intramolecular alkyl C-H bond activation, alcohol dehydrogenation, and trans-cis dihydride isomerization in ruthenium N-heterocyclic carbene complexes [J].
Burling, S ;
Mahon, MF ;
Paine, BM ;
Whittlesey, MK ;
Williams, JMJ .
ORGANOMETALLICS, 2004, 23 (20) :4537-4539
[8]   C-H activation reactions of ruthenium N-heterocyclic carbene complexes: Application in a catalytic tandem reaction involving C-C bond formation from alcohols [J].
Burling, Suzanne ;
Paine, Belinda M. ;
Nama, Devendrababu ;
Brown, Victoria S. ;
Mahon, Mary F. ;
Prior, Timothy J. ;
Pregosin, Paul S. ;
Whittlesey, Michael K. ;
Williams, Jonathan M. J. .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2007, 129 (07) :1987-1995
[9]   Ruthenium induced C-N bond activation of an N-heterocyclic carbene: Isolation of C- and N-bound tautomers [J].
Burling, Suzanne ;
Mahon, Mary F. ;
Powell, Rachael E. ;
Whittlesey, Michael K. ;
Williams, Jonathan M. J. .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2006, 128 (42) :13702-13703
[10]   Easy activation of two C-H bonds of an N-heterocyclic carbene N-methyl group [J].
Cabeza, JA ;
del Río, I ;
Miguel, D ;
Sánchez-Vega, MG .
CHEMICAL COMMUNICATIONS, 2005, (31) :3956-3958
12345678