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首页> 外文期刊>Polyhedron: The International Journal for Inorganic and Organometallic Chemistry >Competitive formation of spiro and ansa derivatives in the reactions of tetrafluorobutane-1,4-diol with hexachlorocyclotriphosphazene: A comparison with butane-1,4-diol
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Competitive formation of spiro and ansa derivatives in the reactions of tetrafluorobutane-1,4-diol with hexachlorocyclotriphosphazene: A comparison with butane-1,4-diol

机译：四氟丁烷-1,4-二醇与六氯环三磷腈的反应中螺和ansa衍生物的竞争形成：与丁烷-1,4-二醇的比较

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摘要

Reaction of hexachlorocyclotriphosphazene, N3P3Cl6 (1), in two stoichiometries (1:1.2 and 1: 3) with the sodium derivative of the fluorinated diol, 2,2,3,3-tetrafluorobutane-1,4-diol (2), in THF solution at room temperature afforded six products, whose structures have been characterized by X-ray crystallography and H-1, F-19 and P-31 NMR spectroscopy: the mono-spiro compound, N3P3Cl4(OCH2CF2CF2CH2O) (3), its ansa isomer (4), a di-spiro derivative N3P3Cl2(OCH2CF2CF2CH2O)(2) (5), its spiro-ansa (6) and non-gem cis bis-ansa (7) isomers and a tri-spiro compound N3P3(OCH2CF2CF2CH2O)(3) (8). The tri-spiro derivative 8 was also formed in the reaction of the ansa compound 4 with diol (2) in a 1:3 ratio in THF at room temperature. The reactions of I with step-wise additions of 2 were also investigated at low temperature (-78 degrees C) to give the same range of products as at room temperature. The results of all reactions are compared with previous work on the reactions of I with butane-1,4-diol/pyridine mixtures and with the reaction of hexafluorocyclotriphosphazene, N3P3F6 (9), with the silyl derivative of the diol (2), (Me3SiOCH2CF2)(2), in a 1:0.4 mole ratio in the same solvent, THF. (c) 2005 Elsevier Ltd. All rights reserved.
机译：六氯环三磷腈N3P3Cl6（1）在两个化学计量比（1：1.2和1：3）中与氟化二醇2,2,3,3-四氟丁烷-1,4-二醇（2）的钠衍生物反应室温下的THF溶液提供六种产品，其结构已通过X射线晶体学以及H-1，F-19和P-31 NMR光谱进行了表征：单螺化合物N3P3Cl4（OCH2CF2CF2CH2O）（3），其ansa异构体（4），双螺环衍生物N3P3Cl2（OCH2CF2CF2CH2O）（2）（5），螺-螺氨基苯甲酸（6）和非-gem cis bis-ansa（7）异构体和三螺环化合物N3P3（OCH2CF2CF2CH2O） （3）（8）。在室温下，ansa化合物4与二醇（2）在THF中以1：3的比例反应也形成了三螺衍生物8。还研究了在低温（-78摄氏度）下I逐步加入2的反应，得到了与室温相同的产物范围。将所有反应的结果与之前关于I与1,4-丁二醇/吡啶混合物的反应以及六氟环三磷腈N3P3F6（9）与二醇的甲硅烷基衍生物（2）的反应进行比较，（ Me3SiOCH2CF2）（2）在相同溶剂THF中的摩尔比为1：0.4 （c）2005 Elsevier Ltd.保留所有权利。

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