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Automated structure verification based on a combination of 1D 1H NMR and 2D 1H13C HSQC spectra

✍ Scribed by Sergey S. Golotvin; Eugene Vodopianov; Rostislav Pol; Brent A. Lefebvre; Antony J. Williams; Randy D. Rutkowske; Timothy D. Spitzer

Publisher: John Wiley and Sons
Year: 2007
Tongue: English
Weight: 360 KB
Volume: 45
Category: Article
ISSN: 0749-1581
DOI: 10.1002/mrc.2034

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✦ Synopsis

Abstract

A method for structure validation based on the simultaneous analysis of a 1D ^1^H NMR and 2D ^1^H^13^C single‐bond correlation spectrum such as HSQC or HMQC is presented here. When compared with the validation of a structure by a 1D ^1^H NMR spectrum alone, the advantage of including a 2D HSQC spectrum in structure validation is that it adds not only the information of ^13^C shifts, but also which proton shifts they are directly coupled to, and an indication of which methylene protons are diastereotopic. The lack of corresponding peaks in the 2D spectrum that appear in the 1D ^1^H spectrum, also gives a clear picture of which protons are attached to heteroatoms. For all these benefits, combined NMR verification was expected and found by all metrics to be superior to validation by 1D ^1^H NMR alone. Using multiple real‐life data sets of chemical structures and the corresponding 1D and 2D data, it was possible to unambiguously identify at least 90% of the correct structures. As part of this test, challenging incorrect structures, mostly regioisomers, were also matched with each spectrum set. For these incorrect structures, the false positive rate was observed as low as 6%. Copyright © 2007 John Wiley & Sons, Ltd.

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