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化学学报
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化学学报 ›› 2005, Vol. 63 ›› Issue (20): 1931-1935. 上一篇    下一篇

研究简报

单取代多金属氧酸盐有机亚胺衍生物(n-Bu4N)2[Mo6O18(≡NAr)] (Ar＝o-CH3OC6H4)的合成

夏芸1，魏永革*,2,3，郭洪猷*,1   

  1. (1北京化工大学理学院 北京 100029)
    (2北京大学化学与分子工程学院 分子动态与稳态结构国家重点实验室 北京 100871)
    (3清华大学化学系 北京 100084)
  • 投稿日期:2005-03-03 修回日期:2005-06-20 发布日期:2010-12-10
  • 通讯作者: 魏永革

Monofunctionalized Organoimido Derivative of the Polyoxometalate: Synthesis of (n-Bu4N)2[Mo6O18(≡NAr)] (Ar＝o-CH3OC6H4)

XIA Yun1, WEI Yong-Ge*,2,3, GUO Hong-You*,1   

  1. (1 Beijing University of Chemical Technology, Beijing 100029)
    (2 College of Chemistry and Molecular Engineering, Peking University, Beijing 100871)
    (3 Department of Chemistry, Tsinghua University, Beijing 100084)
  • Received:2005-03-03 Revised:2005-06-20 Published:2010-12-10
  • Contact: WEI Yong-Ge

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采用N,N'-二环已基碳酰亚胺(DCC)脱水法, 以(n-Bu4N)2[Mo6O19]∶DCC∶邻甲氧基苯胺＝1.5∶1.1∶1.0的摩尔比, 无水乙腈中加热回流12 h, 通过丙酮/乙醇溶液重结晶两次, 得到橘红色片状晶体. 探讨了最佳反应条件: DCC的量在1.0～1.1 mmol, 反应时间12 h. 通过元素分析, UV/Vis光谱和1H NMR谱的研究表明, 该晶体是一种新的六钼酸盐的有机亚胺衍生物 (n-Bu4N)2[Mo6O18(≡NAr)] (Ar＝o-CH3OC6H4).

关键词: 多金属氧酸盐, 有机亚胺衍生物, DCC脱水法, 超分子组装

(n-Bu4N)2 [Mo6O18(≡NAr)] (Ar＝o-CH3OC6H4) was synthesized from a reaction of of hexa- molybdate (2.05 g, 1.5 mmol), o-anisidine (0.11 mL, 1.0 mmol) and DCC (0.23 g, 1.1 mmol) in anhydrous acetonitrile at 100 ℃ for 12 h, where DCC is a dehydrating agent. The nacarat lamellar compounds were recrystallized in the mixed solution of acetone and ethanol with the volume ratio of 2∶1. After studying its UV/Vis, 1H NMR spectroscopy and element analysis, the compound is confirmed to be a new monofunctionalized arylimido derivative of hexamolybdate.

Key words: polyoxometalate, organoimido derivative, DCC, supramolecular assembly