Olivera Cvetković, Johannes Theiner, Mariusz J. Wolff, Kai Hultzsch
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引用次数: 0
摘要
研究了[ReOCl3(PPh3)2]对邻甲苯胺、间甲苯胺、邻氟苯胺、间氟苯胺、对溴苯胺、对氯苯胺和对甲氧基苯胺的反应性，并得到了新型铼（V）亚氨基配合物[Re(NC6H4R)Cl3(PPh3)2]（R = o-Me、m-Me、o-F、m-F、p-Cl、p-Br、p-OMe）。所得产物的表征方法包括元素分析、电喷雾离子化高分辨质谱（ESI-HRMS）、1H、13C{1H}、19F{1H} 和 31P{1H} NMR、傅立叶变换红外光谱（FT-IR）。核磁共振、傅立叶变换红外光谱和 X 射线晶体学。对于间甲苯胺、间氟苯胺和对氯苯胺，铼（V）亚氨基单核[Re(NC6H4R)Cl3(H2NC6H4R)(PPh3)]（R = m-F，p-Cl）配合物和双核[{Re(m-NC6H4Me)Cl2(m-H2NC6H4Me)(PPh3)}2O]配合物作为副产品被分离出来，并通过 X 射线晶体学进行了表征。所有六配位铼（V）络合物都显示出扭曲的八面体配位几何。
Reactivity of [ReOCl3(PPh3)2] towards substituted anilines
The reactivity of [ReOCl3(PPh3)2] towards o-toluidine, m-toluidine, o-fluoroaniline, m-fluoroaniline, p-bromoaniline, p-chloroaniline and p-anisidine was examined and novel rhenium(V) imido complexes [Re(NC6H4R)Cl3(PPh3)2] (R = o-Me, m-Me, o-F, m-F, p-Cl, p-Br, p-OMe) were obtained. The resulting products were characterized by elemental analysis, electrospray ionization high-resolution mass spectrometry (ESI-HRMS), 1H, 13C{1H}, 19F{1H} and 31P{1H} NMR, FT-IR spectroscopy, and X-ray crystallography. For m-toluidine, m-fluroaniline and p-chloroaniline, rhenium(V) imido-amino mononuclear [Re(NC6H4R)Cl3(H2NC6H4R)(PPh3)] (R = m-F, p-Cl) complexes and binuclear [{Re(m-NC6H4Me)Cl2(m-H2NC6H4Me)(PPh3)}2O] complex were isolated as side products and characterized by X-ray crystallography. All six-coordinate rhenium(V) complexes display distorted octahedral coordination geometry.
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