Synthesis and Characterization of Phenoxyphosphazenes. Structure of 2,2-[2,2′-metheylenebis(4-chlorophenoxy)]-4,4,6,6-tetrachlorocyclo-2λ5,4λ5,6λ5-triphosphazatriene (Spiro)

Abstract

The reactions of trimericphosphazenes with sodium [2, 2′- methylenebis(4-chlorophenoxide)] have been investigated. Experimental studies were carried out in argon atmosphere. The sodium aryloxides were prepared from methylenebis (4-chlorophenol) and sodium. The phosphazene and phenolate were reacted at -20°C and then refluxed. After the reaction products (1 and 2) were separated by column chromatography, the structures of the compounds were characterized by elemental analysis, IR, 1H-, 13C-, 31P-NMR, and mass spectroscopy. The compound 1 (spiro) crystallizes in the monoclinic space group Cm with unit cell parameters: a=8.231(1), b=16.242(2), c=7.731(1) Å, β=103.31(1)°, V=1005.8(2) Å3, D<inf>x</inf>=1.796 g cm-3 respectively. The crystal structures were solved by direct methods and refined by full-matrix least squares. © 2005 Elsevier B.V. All rights reserved.