✦ LIBER ✦

Synthesis of a tritium labelled phospholipase A2 inhibitor: A ligand for macromolecular 3H NMR spectroscopy

✍ Scribed by A. S. Culf; H. Morimoto; P. G. Williams; W. J. S. Lockley; W. U. Primrose; J. R. Jones

Publisher: John Wiley and Sons
Year: 1996
Tongue: French
Weight: 490 KB
Volume: 38
Category: Article
ISSN: 0022-2135
DOI: 10.1002/(sici)1099-1344(199604)38:4<373::aid-jlcr844>3.0.co;2-u

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✦ Synopsis

A tritium labelled phospholipase A2 (PLA2) amide analogue inhibitor was prepared by the reduction of an alkene precursor. Diimide, heterogeneous and homogeneous metal catalyzed reduction methods were assessed for their suitability for the preparation of a tritiated ligand for 3H NMR spectroscopic studies. The chosen homogeneous metal-catalyzed method gave a product of specific activity 57 Ci mmol-1, which was isolated by flash chromatography. The binding of this tritiated substrate to bovine pancreatic PLA2 was observed by 3H NMR spectroscopy in the presence of calcium ions. Chemical shift changes suggest that the tritium atoms are located within the hydrophobic pocket of the protein, close to two phenyldanine residues.

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