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The Synthesis and 31P NMR Spectral Studies of Cyclophosphazenes
Authors:Le Wang  Yong Ye  Zhiyu Ju  Shangbin Zhong  Yufen Zhao
Affiliation:1. Key Laboratory of Chemical Biology and Organic Chemistry of Henan Province, Department of Chemistry , Zhengzhou University , Zhengzhou, China;2. Key Laboratory of Chemical Biology and Organic Chemistry of Henan Province, Department of Chemistry , Zhengzhou University , Zhengzhou, China;3. Key Laboratory of Bioorganic Phosphorus Chemistry &4. Chemical Biology (Ministry of Education), Department of Chemistry , Tsinghua University , Beijing, China;5. Chemical Biology (Ministry of Education), Department of Chemistry , Tsinghua University , Beijing, China;6. Department of Chemistry and Key Laboratory for Chemical Biology of Fujian Province , Xiamen University , Xiamen, China
Abstract:A modified method for preparing large-scale quantities of pure hexachlorocyclophosphazene (N3P3Cl6) and octachlorocyclotetraphosphazene (N4P4Cl8), phosphorus pentachloride with ammonium chloride, in the presence of zinc chloride, has been developed. The time of the reaction and the quantities of the catalyst are also studied. It is found that the optimum reaction time is 1.5 h and by-products are remarkably reduced by addition of 10% zinc chloride. As indicated by the 31 P NMR spectra, the synthesis and separation of cyclophosphazenes can be accomplished in moderate yield of tetramer (39%) and good yield of trimer (83%).
Keywords:Cyclophosphazenes  31P NMR  pyridine  synthesis  zinc chloride
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