Facile One-Step Synthesis of MPHMes from MesPCl2 (M = Li, Na, K; Mes = 2,4,6-Me3C6H2)
journal contributionposted on 15.04.2013, 00:00 by Ivana Jevtovikj, Rebeca Herrero, Santiago Gómez-Ruiz, Peter Lönnecke, Evamarie Hey-Hawkins
Reaction of alkali metals (Li, Na, K) with mesityldichlorophosphane (MesPCl2, Mes = 2,4,6-Me3C6H2) in ethereal solvents leads to formation of the corresponding mesitylphosphanides MPHMes in good purity and yield. 31P NMR spectroscopic studies in deuterated solvents strongly support a mechanism of the reaction that involves protonation/disproportionation steps in which the solvent is the only possible proton source. Li(thf)(tmeda)PHMes (1), [Na(tmeda)(μ-PHMes)]∞ (2), and [K(pmdeta)(μ-PHMes)]2 (3) (tmeda = N,N,N′,N′-tetramethylethylenediamine, pmdeta = N,N,N′,N″,N″-pentamethyldiethylenetriamine) were obtained; in the solid state, 2 forms zigzag chains while 3 is a dimeric compound.