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Application of 1D BIRD or X-filtered DEPT long-range C-C relay for detection of proton and carbon via four bonds and measuring long-range C-13-C-13 coupling constants

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タイトル: Application of 1D BIRD or X-filtered DEPT long-range C-C relay for detection of proton and carbon via four bonds and measuring long-range C-13-C-13 coupling constants
著者: Fukushi, Eri 著作を一覧する
Kawabata, Jun 著作を一覧する
キーワード: NMR
H-1
C-13
C-13-detecting 1D X-filtered DEPT long-range C-C relay
1D BIRD-DEPT long-range C-C relay
long-range C-13-C-13 coupling constants
発行日: 2006年 1月 5日
出版者: John Wiley & Sons
誌名: Magnetic Resonance in Chemistry
巻: 44
号: 4
開始ページ: 475
終了ページ: 480
出版社 DOI: 10.1002/mrc.1768
抄録: We propose the C-13-detecting 1D DEPT long-range C-C relay to detect super long-range H-C connectivity via four bonds (H-1-C-13-X-X-C-13, X represents C-12 or heteronuclear). It is derived from the DEPT C-C relay which detects the H-C correlations via two bonds (H-1-C-13-C-13) by setting the delays for J(CC) in the C-C relay sequence to the (LR)J(CC). This sequence gives correlation signals split by small (LR)J(CC), which seriously suffers from residual center signal. The unwanted signal is due to long-range C-H couplings ((LR)J(CH)). The expected relayed magnetization transfer (1)J(CH) -> (LR)J(CC) occurs in the H-1-C-13-X-(X)-C-13 isotopomer, whereas the unwanted signal of (LR)J(CH) comes from H-1-C-12-(X)-C-13 isotopomers, whose population is 100 times larger than that of the H-1-C-13-X-(X)-C-13 isotopomer. The large dispersive line of this unwanted center signal would be a fatal problem in the case of detecting small (LR)J(CC) couplings. This central signal could be removed by an insertion of BIRD pulse or X-filter. DEPT spectrum editing solved a signal overlapping problem and enabled accurate determination of particular (LR)J(CC) values. We demonstrate here the examples of structure determination using connectivity between H-1 and C-13 via four bonds, and the application of long-range C-C coupling constants to discrimination of stereochemical assignments.
Rights: Copyright © 2006 John Wiley & Sons, Ltd.
関連URI: http://www3.interscience.wiley.com/cgi-bin/jhome/3767
資料タイプ: article (author version)
URI: http://hdl.handle.net/2115/8469
出現コレクション:雑誌発表論文等 (Peer-reviewed Journal Articles, etc)

提供者: 福士 江里

 

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