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1JCC‐edited HSQC‐1,n‐ADEQUATE: a new paradigm for simultaneous direct and long‐range carbon–carbon correlation
Authors:Gary E Martin  Kirill A Blinov  Mikhail Reibarkh  R Thomas Williamson
Institution:1. Discovery and Preclinical Sciences, Process & Analytical Chemistry – Structure Elucidation Group, Merck Research Laboratories, Summit, NJ 07901, USA, Merck Research Laboratories, , Summit, NJ, 07901 USA;2. Molecule Apps, LLC, , Moscow, 123181 Russian Federation;3. Discovery and Preclinical Sciences, Process & Analytical Chemistry – Structure Elucidation Group, Merck Research Laboratories, , Rahway, NJ, 07065 USA
Abstract:Establishing the carbon skeleton of a molecule greatly facilitates the process of structure elucidation, leaving only heteroatoms to be inserted, heterocyclic rings to be closed, and stereochemical features to be defined. INADEQUATE, and more recently PANACEA, have been the only means of coming close to the goal of totally defining the carbon skeleton of a molecule. Unfortunately, the extremely low sensitivity and prodigious sample requirements of these experiments and the multiple receiver requirement for the latter experiment have severely restricted the usage of these experiments. Proton‐detected ADEQUATE experiments, in contrast, have considerably higher sensitivity and more modest sample requirements. By combining experiments such as 1,1‐ADEQUATE and 1,n‐ADEQUATE with higher sensitivity experiments such as GHSQC through covariance processing, sample requirements can be further reduced with a commensurate improvement in the s/n ratio and F1 resolution of the covariance processed spectrum. We now wish to report the covariance processing of an inverted 1JCC 1,n‐ADEQUATE experiment with a non‐edited GHSQC spectrum to afford a spectrum that can trace the carbon skeleton of a molecule with the exception of correlations between quaternary carbons. Copyright © 2012 John Wiley & Sons, Ltd.
Keywords:covariance processing  1  n‐ADEQUATE  inverted 1JCC 1  n‐ADEQUATE  HSQC‐1  n‐ADEQUATE  1JCC‐edited HSQC‐1  n‐ADEQUATE
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