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Applications of 1,1-adequate

NM160002E

1,1-adequate is a technique to obtain heteronuclear correlation similarly to hmbc. While correlation signals from hmbc do not separate 2JCH from 3JCH, 1,1-adequate, which exclusively observes 1JCH amd 2JCH, can be combined with hsqc to identify 2JCH. 1,1-adequate uses 1JCH and 1JCC coupling for signal observation. This technique is effective for compounds rich in quaternary carbon and for aromatic ring identification.
1,1-adequateのパルスシーケンス
1,1-adequate signal emergence

1,1-adequate is not high in sensitivity because it uses 1JCC for signal observation. However, being an inverse analysis on the 1H side, 1,1-adequate is capable of higher sensitivity analysis than inadequate.
For measurement conditions, parameters for1JCH and 1JCC are defined.

100 mg 4-methylumbelliferone/DMSO-d6
Shown below are total and magnified views of 1,1-adequate.



Instruments used: JNM-ECZ400S+ROYAL probe
Measuring conditions: 48 scans (7h), J_constant=140 Hz, JCC=60 Hz

Reference

B. Reif, M. Kock, R. Kerssebaum, H. Kang, W. Fenical, C. Griesinger, JMR ser-A 1996, 118, 282-285 M. Kock, R. Kerssebaum, W. Bermel, MRC 2003, 41, p65-69

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