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有机化学
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有机化学 ›› 1995, Vol. 15 ›› Issue (2): 194-201. 上一篇    下一篇

研究论文

[η^5-Bz~5C~5(CO)~nM]~2的合成

宋礼成;王吉泉;张鲁岩;胡青眉;黄小荣   

  1. 南开大学化学系;中国科学院福建物质结构研究所结构化学国家;验室
  • 发布日期:1995-04-25

Syntheses and structures of dinuclear molybdenum and tungsten compounds containing η^5-pentabenzylcyclopentadienyl ligand [η^5-Bz~5C~5(CO)~nM]~2 (M=Mo, n=2,3; M=W, n=3)

SONG LICHENG;ZHANG LUYAN;HU QINGMEI;HUANG XIAORONG   

  • Published:1995-04-25

本文通过η^5-Bz~5C~5MNa与氧化偶联试剂Fe~2(SO~4)~3/HOAC/H~2O的反应合成了含η^5-五苄基环戊二烯基配体的两个金属-金属单键化合物[η^5-Bz~5C~5(CO)~3M]~2 (1: M=Mo; 2: M=W) , 产率分别为45%和19% . 1 在沸腾的甲苯中可进一步脱碳而以98%的产率生成金属-金属叁键化合物[η^5-Bz~5C~5(CO)~2Mo]~2 (3).1～3的结构均经碳氢分析, IR, ^1H NMR 和MS鉴定. 3的结构尚被单晶X射线衍射分析确证 .

关键词: 双核络合物, 钼化合物, 合成晶体结构, 环戊二烯基, 钨化合物

Two metal-metal singly bonded compounds containing η^5-pentabenzlcyclopen tadienyl ligand [η^5-Bz~5C~5(CO)~3M]~2 (1 M=Mo , 2 M=W) were synthesized in 45% and 19% yield through the reaction of η^5Bz~5C~5(CO)~3 M Na with a combined oxidative reagent Fe~2(SO~4)~3/HOAc/H~2O . Further decarbonylation of 1 in refluxing toluene gave the metal-metal triply bonded compound [η^5-Bz~5C~5(CO)~2Mo]~2 (3) in 98% yield. The structures of 1～3 were characterized by C/H analysis IR, ^1H NMR and MS spectroscopies. The structure of 3 were characterized by C/H analysis IR,^1H NMR and MS spectroscopies. The structure of 3 was further confirmed by single-crystal X-ray diffraction analysis.

Key words: DINUCLEAR COMPLEX, MOLYBDENUM COMPOUNDS, CYCLOPENTADIENYL GROUP, TUNGSTEN COMPOUNDS

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