Using signal amplification by reversible exchange (SABRE) to hyperpolarise 119 Sn and 29 Si NMR nuclei.

Autor: Olaru AM; Department of Chemistry, University of York, Heslington, York YO10 5DD, UK. simon.duckett@york.ac.uk., Burt A; Department of Chemistry, University of York, Heslington, York YO10 5DD, UK. simon.duckett@york.ac.uk., Rayner PJ; Department of Chemistry, University of York, Heslington, York YO10 5DD, UK. simon.duckett@york.ac.uk., Hart SJ; Department of Chemistry, University of York, Heslington, York YO10 5DD, UK. simon.duckett@york.ac.uk., Whitwood AC; Department of Chemistry, University of York, Heslington, York YO10 5DD, UK. simon.duckett@york.ac.uk., Green GGR; Department of Chemistry, University of York, Heslington, York YO10 5DD, UK. simon.duckett@york.ac.uk., Duckett SB; Department of Chemistry, University of York, Heslington, York YO10 5DD, UK. simon.duckett@york.ac.uk.
Jazyk: angličtina
Zdroj: Chemical communications (Cambridge, England) [Chem Commun (Camb)] 2016 Dec 13; Vol. 52 (100), pp. 14482-14485.
DOI: 10.1039/c6cc07109k
Abstrakt: The hyperpolarisation of the 119 Sn and 29 Si nuclei in 5-(tributylstannyl)pyrimidine (A Sn ) and 5-(trimethylsilyl)pyrimidine (B Si ) is achieved through their reaction with [IrCl(COD)(IMes)] (1a) or [IrCl(COD)(SIMes)] (1b) and parahydrogen via the SABRE process. 1a exhibits superior activity in both cases. The two inequivalent pyrimidine proton environments of A Sn readily yielded signal enhancements totalling ∼2300-fold in its 1 H NMR spectrum at a field strength of 9.4 T, with the corresponding 119 Sn signal being 700 times stronger than normal. In contrast, B Si produced analogous 1 H signal gains of ∼2400-fold and a 29 Si signal that could be detected with a signal to noise ratio of 200 in a single scan. These sensitivity improvements allow NMR detection within seconds using micromole amounts of substrate and illustrate the analytical potential of this approach for high-sensitivity screening. Furthermore, after extended reaction times, a series of novel iridium trimers of general form [Ir(H) 2 Cl(NHC)(μ-pyrimidine-κN:κN')] 3 precipitate from these solutions whose identity was confirmed crystallographically for B Si .
Databáze: MEDLINE
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