TRIMETHYLPHOSPHINE-SILVER IODIDE COMPLEX

Purification Methods

It is decomposed by heating gently in one arm of an inverted U tube. The other arm is kept in a freezing mixture. The complex dissociates, and pure Me3P collects in the cold arm and is used at once. It should not be allowed to come in contact with air [for AsMe3 see Mann & Wells J Chem Soc 708 1938]. The CS2 complex has m 119o (crystallising from 95% EtOH) and decomposes in CCl4 to give Me3PS m 154o (from EtOH) [Sorettas & Isbell J Org Chem 27 273 1962]. Trimethylphosphine hydrochloride is unstable and volatilises at 75o/0.4mm (120o/14mm). [Brown J Am Chem Soc 67 503 1945, IR: Wagstaffe & Thompson Trans Faraday Soc 40 41 1944, Kosolapoff Organo-phosphorus Compounds, Wiley p 31 1950, Beilstein 4 IV 3429.]