高等学校化学学报

高等学校化学学报 ›› 1998, Vol. 19 ›› Issue (1): 70.

• 论文 • 上一篇    下一篇

三(三甲基硅)环戊二烯与六羰基钼的反应

徐善生, 龚军芳, 周秀中   

  1. 南开大学化学系, 天津, 300071
  • 收稿日期:1996-12-20 出版日期:1998-01-24 发布日期:1998-01-24
  • 通讯作者: 周秀中
  • 作者简介:徐善生,男,54岁,副教授.
  • 基金资助:

    国家自然科学基金及国家教育委员会博士学科点基金资助课题.

The Reaction of Tris(trimethylsilyl) cyclopentadiene with Hexacarbonyl Molybdenum

XU Shan-Sheng, GONG Jun-Fang, ZHOU Xiu-Zhong   

  1. Department of Chemistry, Nankai University, Tianjin, 300071
  • Received:1996-12-20 Online:1998-01-24 Published:1998-01-24

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被引次数

4

摘要： 三(三甲基硅)环戊二烯与六羰基钼在二甲苯中回流8h,反应停留在生成中间物η5-[(Me3Si)NC5H5-n]Mo(CO)3H(n=2,3)(I)的阶段.不经分离,I随即分别与CCl4·NBS及MeI反应,生成其相应的钼卤化物η-5[(Me3Si)NC5H5-n]Mo(CO)3X[n=3,X=Cl(1),Br(2),I(3);n=2,X=Cl(4),Br(5),I(6)].4-6是由于茂环上脱掉1个Me3Si基.经元素分析和IR及1H NMR谱表征了化合物1-6的结构,并用X射线衍射测定了1的晶体结构.

关键词: 双核钼化合物, 钼氢化物, 脱硅基作用, 晶体结构

Abstract: The xylene solution of tris (trimethylsilyl)cyclopentadiene and Mo(CO)6 was refluxed for 8 h. The reaction was stopped at the formation of the intermediate, mononuclear molybdenum hydride η5-[(Me3Si)nC5H5-n]Mo (CO)3H (n=2, 3) (Ⅰ). The reaction can not proceed further to form the binuclear(Mo-Mo) product. It is probably due to the steric effect of three silyl groups which hindered the further progress of the reaction. Desilylation happened while the reaction was proceeding. Compound Ⅰ was not isolated from the xylene solution and reacted immediately with CCl4, NBS and MeI respectively to give the corresponding molybdenum halides η5-[(Me3Si)nC5H5-n]Mc (CO)3,X [n=3; X: Cl(1), Br(2), I(3). n=2; X: Cl(4), Br(5), I(6)]. Compounds 4, 5, and 6 are desilylation products. The molecular structures of 1-6 were characterized by elemental analyses, IR and 1H NMR spectra. The crystal structure of 1 was determined by X-ray diffraction.

Key words: Binuclear molybdenum compound, Molybdenum hydride, Desilylation, Crystal structure

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