Preparation
Involves reaction of triphenylphosphine
with 2-(trimethylsilyl)ethoxymethyl chloride in benzene at gentle
reflux for 18 h. Upon cooling, the resulting phosphonium salt
can be recovered by filtration and purified by triturating with
diethyl ether in 94% yield.
Purification Methods
Wash the solid with AcOH and recrystallise it from CH2Cl2/EtOAc. Dry it in a vacuum desiccator. Hygroscopic. 1H NMR (CDCl3) : -0.2 (s, Me3Si), 0.8 (t, 8Hz, CH2Si), 3.83 (t, 8Hz, OCH2), 5.77 (d, JPH 4Hz, P+-CH2O) and 7.70 (m, aromatic H). [Sch.nauer & Zbiral Justus Liebigs Ann Chem 1039 1983.]
