Reversible Hyperpolarization of Ketoisocaproate Using Sulfoxide-containing Polarization Transfer Catalysts.

Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry
Ben J TicknerSimon B Duckett

Abstract

The substrate scope of sulfoxide-containing magnetisation transfer catalysts is extended to hyperpolarize α-ketoisocaproate and α-ketoisocaproate-1-[13 C]. This is achieved by forming [Ir(H)2 (κ2 -ketoisocaproate)(N-heterocyclic carbene)(sulfoxide)] which transfers latent magnetism from p-H2 via the signal amplification by reversible exchange (SABRE) process. The effect of polarization transfer field on the formation of enhanced 13 C magnetization is evaluated. Consequently, performing SABRE in a 0.5 μT field enabled most efficient magnetisation transfer. 13 C NMR signals for α-ketoisocaproate-1-[13 C] in methanol-d4 are up to 985-fold more intense than their traditional Boltzmann derived signal intensity (0.8 % 13 C polarisation). Single crystal X-ray diffraction reveals the formation of the novel catalyst decomposition products [Ir(μ-H)(H)2 (IMes)(SO(Ph)(Me)2 )]2 and [(Ir(H)2 (IMes)(SO(Me)2 ))2 (μ-S)] when the sulfoxides methylphenylsulfoxide and dimethylsulfoxide are used respectively.

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Citations

Aug 3, 2021·Physical Chemistry Chemical Physics : PCCP·Ben J TicknerVille-Veikko Telkki

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Methods Mentioned

BETA
NMR
X‐ray

Software Mentioned

SABRE

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