“Direct” <sup>13</sup>C Hyperpolarization of <sup>13</sup>C‐Acetate by MicroTesla NMR Signal Amplification by Reversible Exchange (SABRE)

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  • Max E. Gemeinhardt
    Department of Chemistry and Biochemistry Southern Illinois University Carbondale IL 62901 USA
  • Miranda N. Limbach
    Department of Chemistry and Biochemistry Southern Illinois University Carbondale IL 62901 USA
  • Thomas R. Gebhardt
    Department of Chemistry and Biochemistry Southern Illinois University Carbondale IL 62901 USA
  • Clark W. Eriksson
    Department of Biomedical Engineering University of Virginia Charlottesville VA USA
  • Shannon L. Eriksson
    Department of Chemistry Duke University Durham NC USA
  • Jacob R. Lindale
    Department of Chemistry Duke University Durham NC USA
  • Elysia A. Goodson
    Carbondale Community High School Carbondale IL 62901 USA
  • Warren S. Warren
    Department of Chemistry Duke University Durham NC USA
  • Eduard Y. Chekmenev
    Department of Chemistry Karmanos Cancer Institute (KCI) Integrative Biosciences (Ibio) Wayne State University Detroit MI 48202 USA
  • Boyd M. Goodson
    Department of Chemistry and Biochemistry Southern Illinois University Carbondale IL 62901 USA

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<jats:title>Abstract</jats:title><jats:p>Herein, we demonstrate “direct” <jats:sup>13</jats:sup>C hyperpolarization of <jats:sup>13</jats:sup>C‐acetate via signal amplification by reversible exchange (SABRE). The standard SABRE homogeneous catalyst [Ir‐IMes; [IrCl(COD)(IMes)], (IMes=1,3‐bis(2,4,6‐trimethylphenyl), imidazole‐2‐ylidene; COD=cyclooctadiene)] was first activated in the presence of an auxiliary substrate (pyridine) in alcohol. Following addition of sodium 1‐<jats:sup>13</jats:sup>C‐acetate, parahydrogen bubbling within a microtesla magnetic field (i.e. under conditions of SABRE in shield enables alignment transfer to heteronuclei, SABRE‐SHEATH) resulted in positive enhancements of up to ≈100‐fold in the <jats:sup>13</jats:sup>C NMR signal compared to thermal equilibrium at 9.4 T. The present results are consistent with a mechanism of “direct” transfer of spin order from parahydrogen to <jats:sup>13</jats:sup>C spins of acetate weakly bound to the catalyst, under conditions of fast exchange with respect to the <jats:sup>13</jats:sup>C acetate resonance, but we find that relaxation dynamics at microtesla fields alter the optimal matching from the traditional SABRE‐SHEATH picture. Further development of this approach could lead to new ways to rapidly, cheaply, and simply hyperpolarize a broad range of substrates (e.g. metabolites with carboxyl groups) for various applications, including biomedical NMR and MRI of cellular and in vivo metabolism.</jats:p>

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