Simultaneous characterization of a mixture of fluorochemicals using three-dimensional 19F-1H heteronuclear TOCSY filtered/edited NMR experiments

被引:13
|
作者
Hu, Haitao [1 ]
Kulanthaivel, Palaniappan [1 ]
Krishnamurthy, Krish [1 ]
机构
[1] Eli Lilly & Co, Discovery Chem Res & Technol & Drug Disposit, Indianapolis, IN 46285 USA
来源
JOURNAL OF ORGANIC CHEMISTRY | 2007年 / 72卷 / 16期
关键词
D O I
10.1021/jo070658w
中图分类号
O62 [有机化学];
学科分类号
070303 ; 081704 ;
摘要
Heteronuclear F-19-H-1 cross-polarization can be used effectively as a tool for both spectral filtering and editing in the NMR analysis of the increasing number of fluorine-containing compounds encountered in drug discovery. Combined with LC-MS, three-dimensional F-19-H-1 heteronuclear TOCSY filtered experiments based on this approach have enabled the simultaneous identification of a mixture of closely related dexamethasone derivatives without the need for isolation.
引用
收藏
页码:6259 / 6262
页数:4
相关论文
共 28 条
  • [1] Simultaneous 19F-1H medium resolution NMR spectroscopy for online reaction monitoring
    Zientek, Nicolai
    Laurain, Clement
    Meyer, Klas
    Kraume, Matthias
    Guthausen, Gisela
    Maiwald, Michael
    JOURNAL OF MAGNETIC RESONANCE, 2014, 249 : 53 - 62
  • [2] Conformational Analysis of Fluorinated Pyrrolidines Using 19F-1H Scalar Couplings and Heteronuclear NOEs
    Combettes, Lorraine E.
    Clausen-Thue, Philip
    King, Michael A.
    Odell, Barbara
    Thompson, Amber L.
    Gouverneur, Veronique
    Claridge, Tim D. W.
    CHEMISTRY-A EUROPEAN JOURNAL, 2012, 18 (41) : 13133 - 13141
  • [3] Applications of broadband 19F-1H cross-polarization in NMR spectroscopy: Hetero-TOCSY and ASAP-HSQC
    Marchione, Alexander
    Diaz, Elizabeth
    ABSTRACTS OF PAPERS OF THE AMERICAN CHEMICAL SOCIETY, 2019, 258
  • [4] Automated data evaluation and modelling of simultaneous 19F-1H medium-resolution NMR spectra for online reaction monitoring
    Zientek, Nicolai
    Laurain, Clement
    Meyer, Klas
    Paul, Andrea
    Engel, Dirk
    Guthausen, Gisela
    Kraume, Matthias
    Maiwald, Michael
    MAGNETIC RESONANCE IN CHEMISTRY, 2016, 54 (06) : 513 - 520
  • [5] Investigation of soft component mobility in thermoplastic elastomers using homo- and heteronuclear dipolar filtered 1H double quantum NMR experiments
    Bertmer, M
    Gasper, L
    Demco, DE
    Blümich, B
    Litvinov, VM
    MACROMOLECULAR CHEMISTRY AND PHYSICS, 2004, 205 (01) : 83 - 94
  • [6] Achievement of 1H-19F heteronuclear experiments using the conventional spectrometer with a shared single high band amplifier
    Sakuma, Chiseko
    Kurita, Jun-ichi
    Furihata, Kazuo
    Tashiro, Mitsuru
    MAGNETIC RESONANCE IN CHEMISTRY, 2015, 53 (05) : 327 - 329
  • [7] NMR spectral analysis of second-order 19F-19F, 19F-1H and 13C-19F coupling constants in pentafluorobenzene and tetrafluoro-4-(morpholino)pyridine using ANATOLIA
    Edgar, Mark
    Zeinali, Fatemeh
    Mojally, Mariam
    Hughes, Charlotte
    Riaz, Shahzad
    Weaver, George W.
    JOURNAL OF FLUORINE CHEMISTRY, 2019, 224 : 35 - 44
  • [8] Direct measurement of the distance between adjacent guest molecules in a disordered solid inclusion compound using solid-state 19F-1H NMR spectroscopy
    Nordon, A
    Hughes, E
    Harris, RK
    Yeo, L
    Harris, KDM
    CHEMICAL PHYSICS LETTERS, 1998, 289 (1-2) : 25 - 29
  • [9] PROBING BOUND WATER IN PROTEINS USING 2-DIMENSIONAL F-19-H-1 NMR
    CISTOLA, DP
    HALL, KB
    JOURNAL OF CELLULAR BIOCHEMISTRY, 1995, : 70 - 70
  • [10] An approach to the simultaneous quantitative analysis of metabolites in table wines by 1H NMR self-constructed three-dimensional spectra
    Li, Bao Qiong
    Xu, Min Li
    Wang, Xue
    Zhai, Hong Lin
    Chen, Jing
    Liu, Jin Jin
    FOOD CHEMISTRY, 2017, 216 : 52 - 59