A simplified and convenient laboratory-scale preparation of 14N or 15N high molecular weight poly(dichlorophosphazene) directly from PCl5

A simplified and convenient laboratory-scale preparation of 14N or 15N high molecular weight poly(dichlorophosphazene) directly from PCl5
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DOI:
10.1002/chem.200304750
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发表时间:
2003-08-18
影响因子:
4.3
通讯作者:
Presa-Soto, A
Presa-Soto, A
中科院分区:
化学2区
文献类型:
--
作者:
Carriedo, GA;Alonso, FLG;Presa-Soto, A

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本文介绍了一种简便的一锅法合成高分子量聚(二氯磷腈)[NPCl_2](n)或N-15同位素异构体[(NPCl_2)-N-15](n)的THF溶液。[NPCl_2](n)在THF中的溶液通过在K_2CO_3存在下制备而获得,不含聚(四氢呋喃),该溶液可以在K_2CO_3或Cs_2CO_3存在下直接与酚、联酚或甚至HO-CH_2CF_3反应,以在非常简单的后处理之后获得相应的几乎不含氯的聚磷腈衍生物。
A simple and convenient onepot synthesis of THF solutions of high molecular weight poly(dichlorophosphazene) [NPCl2](n), or the N-15 isotopomer [(NPCl2)-N-15](n), starting directly from PCl5 and NH4Cl or (NH4Cl)-N-15 in a solution of 1,2,4-trichlorobenzene in the presence of sulfamic acid and calcium sulfate dihydrate, is described. The solutions of [NPCl2](n) in THF, which are obtained free of poly(tetrahydrofuran) by preparing them in the presence of K2CO3, can be reacted directly with phenols, biphenols, or even HO-CH2CF3 in the presence of K2CO3 Or Cs2CO3 to obtain, after a very simple workup, the corresponding polyphosphazene derivatives almost free of chlorine.