Green Traceless Cleavage from Resin-Bound Selenium and Tellurium and Analysis by 2D 29Si/1H HR-MAS NMR Spectroscopy

Thomas Ruhland; Jakob Torang; Henrik Pedersen; Jens Christian Madsen; Kia Svane Bang

doi:10.1055/s-2005-865311

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Green Traceless Cleavage from Resin-Bound Selenium and Tellurium and Analysis by 2D ²⁹Si/¹H HR-MAS NMR Spectroscopy

Thomas Ruhland*, Jakob Torang, Henrik Pedersen, Jens Christian Madsen, Kia Svane Bang
Medicinal Chemistry Research, H. Lundbeck A/S, 9 Ottiliavej, 2500 Valby, Denmark
Fax: +4536438237; e-Mail: tr@lundbeck.com;

Abstract

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Abstract

A novel protocol for traceless cleavage from resin-bound selenium and tellurium is described. The toxic tributyltin hydride that has been used previously as reagent for cleavage from these resins by homolysis has been replaced by the less-toxic tris(trimethylsilyl)silane and tris(trimethylsilyl)germane. In addition, the remaining resin-bound chalcogenyl silane and germane residues were characterised by the use of high-resolution magic-angle spinning (HR-MAS) 2D ²⁹Si/¹H NMR spectroscopy.

Key words

traceless cleavage - ²⁹Si/¹H HR-MAS NMR - resin-bound selenium and tellurium

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References

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