Abstract
The DeJaeger synthesis of poly(dichlorophosphazene), (NPCl 2)n (1) from P-trichloro-N-(dichlorophosphoryl)monophosphazene, Cl 3P=NP(O)Cl 2 (2) represents an attractive alternative to the ring opening polymerization approach to 1. We have followed the Emsley reaction, i.e. PCl 5 and (NH4)2SO4, under a variety of conditions by 31P NMR spectroscopy. Alternative oxygen atom sources in place of (NH4)2SO4 were also explored. Model reactions to identify specific pathways potentially operating in the formation of 2 when combined with the NMR studies allow for identification of the most probable sequence of steps leading to 2. Conversion of 2 to 1 under different conditions was also examined. Molecular weight was monitored as a function of time by GPC with online direct detection of the diphenoxy derivative, [NP(OC6H5)2]n, of 1. The byproduct of the polymerization of 2 is POCl 3. After conversion of 2 to (RO)3PO, a one step process has been developed for conversion into (RO)3P=NSiMe3, another class of poly(phosphazene) precursors.
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