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However, individual isolation of these species is time\u2010consuming, labor\u2010intensive, and often technically challenging, if not impossible. Here, we present an NMR experimental workflow involving the time\u2010resolved acquisition and processing of multiple types of two\u2010dimensional NMR spectra acquired in tandem using NOAH supersequences on an active reaction. This time\u2010resolved NOAH nonuniform sampling method (TR\u2010NOAH\u2010NUS) enables the generation of robust concentration\u2013time plots for kinetic analysis in parallel to structural characterization of reaction components. Here, we demonstrate the application of TR\u2010NOAH\u2010NUS on an organo\u2010catalyzed acylation of alcohols. Despite the short (30\u2009min) timespan of the reaction, we are able to obtain high\u2010quality HSQC, HMBC, and COSY spectra with excellent (less than 15\u2009s) temporal resolution. From these data, we can observe both an on\u2010cycle catalytic intermediate and an off\u2010cycle catalyst degradation product and can directly assign the structures of both without need for further isolation.<\/jats:p>","DOI":"10.1002\/mrc.70103","type":"journal-article","created":{"date-parts":[[2026,4,6]],"date-time":"2026-04-06T01:11:33Z","timestamp":1775437893000},"page":"621-628","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Integrated Reaction Monitoring and In\u00a0Situ Structural Elucidation of Reactive Intermediates With Time\u2010Resolved NOAH NMR Supersequences"],"prefix":"10.1002","volume":"64","author":[{"ORCID":"https:\/\/orcid.org\/0009-0006-4096-5079","authenticated-orcid":false,"given":"Sara\u00a0M.","family":"Guzman","sequence":"first","affiliation":[{"name":"Department of Chemistry The University of British Columbia  Vancouver British Columbia Canada"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2461-8150","authenticated-orcid":false,"given":"Yael","family":"Ben\u2010Tal","sequence":"additional","affiliation":[{"name":"Department of Chemistry The University of British Columbia  Vancouver British Columbia Canada"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiayu","family":"Zhang","sequence":"additional","affiliation":[{"name":"Department of Chemistry The University of British Columbia  Vancouver British Columbia Canada"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Mark","family":"Dixon","sequence":"additional","affiliation":[{"name":"Mestrelab Research S.L.  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