ic302759k_si_001.pdf (295.23 kB)
Facile One-Step Synthesis of MPHMes from MesPCl2 (M = Li, Na, K; Mes = 2,4,6-Me3C6H2)
journal contribution
posted on 2013-04-15, 00:00 authored by Ivana Jevtovikj, Rebeca Herrero, Santiago Gómez-Ruiz, Peter Lönnecke, Evamarie Hey-HawkinsReaction 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.
