Optimized polarization build-up times in dissolution DNP-NMR using a benzyl amino derivative of BDPA

The synthesis of two novel BDPA-like radicals, a benzyl amino (BAm-BDPA, 7 ) and a cyano (CN-BDPA, 5 ) derivative, is reported and their behaviour as polarizing agents for fast dissolution Dynamic Nuclear Polarization (DNP) is evaluated. The radical 7 is a promising candidate for DNP studies since i...

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Veröffentlicht in:RSC advances 2016-01, Vol.6 (32), p.2777-2782
Hauptverfasser: Muñoz-Gómez, J. L, Monteagudo, E, Lloveras, V, Parella, T, Veciana, J, Vidal-Gancedo, J
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Sprache:eng
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Zusammenfassung:The synthesis of two novel BDPA-like radicals, a benzyl amino (BAm-BDPA, 7 ) and a cyano (CN-BDPA, 5 ) derivative, is reported and their behaviour as polarizing agents for fast dissolution Dynamic Nuclear Polarization (DNP) is evaluated. The radical 7 is a promising candidate for DNP studies since it is soluble in neat [1- 13 C]pyruvic acid (PA), and therefore the use of an additional glassing agent for sample homogeneity is avoided. In addition, a 60 mM sample of 7 offers optimum 13 C NMR signal enhancements using fairly short polarization times (about 1800 s). It is shown that DNP-NMR measurements using 7 can be performed much more efficiently in terms of the signal enhancement per polarization build-up time unit than when using the reference OX63 or BDPA radicals. These enhanced features are translated to a substantial reduction of polarization times that represents an optimum temporary use of the DNP polarizer and allow economized liquid helium consumption. A BAm-BDPA radical has proved to be a quick and efficient polarizing agent, showing optimum 13 C NMR signal enhancements per polarization time unit.
ISSN:2046-2069
2046-2069
DOI:10.1039/c6ra00635c