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High-Yield Synthesis and Crystal Structure Determination of Sodium Triphenylphosphane Monosulfonate (TPPMSNa)

✍ Scribed by Arndt Karschin; Wolfgang Kläui; Wilfried Peters; Bernhard Spingler

Publisher: John Wiley and Sons
Year: 2010
Tongue: English
Weight: 324 KB
Volume: 2010
Category: Article
ISSN: 1434-1948
DOI: 10.1002/ejic.200901002

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✦ Synopsis

Abstract

A simple, high‐yield synthesis is described that leads tothe sodium salt of monosulfonated triphenylphosphane (TPPMS^Na^) as a pure product in large quantities without complicated workup techniques. The single‐crystal X‐ray structure of TPPMS^Na^**·**2.5H~2~O is reported. The structure is built up by alternating layers of aquated sodium sulfonate units and hydrophobic triphenyl units. Thermogravimetric analyses show the loss of one molecule of water at 70 and one at 105 °C. Thermal decomposition occurs at temperatures above 400 °C. The anhydrous ligand is hygroscopic. The preparation of the free acid TPPMS^H^ starting from the sodium salt is also reported. TPPMS^H^ is an extremely hygroscopic solid that could not be isolated in the crystalline form.

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