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金属有机化合物的分析(Ⅸ)双(烯基环戊二烯基)钛、锆、铪二卤、二硫氰基、二巯基化合物的纸色谱研究

Analysis of Organometallic Compounds. Ⅸ. Paper Chromatography of Bis(alkenyicydopentadienyl)Titanium, Zirconium and Halfnium Dichlorides,Dithiocyanato and Dimercaprto Derivatives

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【作者】 李松兰杨学谨李云鹏杜一涓陈寿山

【Author】 Li Songtan, Yang Xuejin, Li Yunpeng & Du Yijuan, Department of Chemistry, Nankai,University, Tianjin; Chen Shoushan, Institute of Element-Organic Chemistry, Nankai University,Tianjin

【机构】 南开大学化学系南开大学元素有机化学研究所 天津天津天津

【摘要】 本文用纸色谱法对(R-Cp)2MX2 类化合物(R=各种烯基,M=Ti,Zr,Hf,X=F,Cl,Br,SCN,SH)进行分离,用磷酸酯类,癸烷:磷酸三丁酯=1:1或1:2作展开剂,有效地分离了R相同、X相同、M不同的化合物,呈RfTi>RfZr>RfHf的规律。也成功地分离了R相同、M相同、X不同的化合物,呈RfF>RfBr>RfCl的规律。用磷酸酯类作展开剂可分离B相同,M=Ti,X=Cl,SCN 的化合物以及X=Cl,SH的化合物,呈Rfcl>RfSCN以及Rfcl>RfSH的规律。以癸烷为稀释剂可增加分离效果,随稀释剂量增加,化合物Rf值降低。

【Abstract】 Papar chromatography has been successfully used for the separaton of a series of compounds represented by the formula (R-Cp)2MX2(R= various alkenyl. M=Ti, Zr, Hf, X=F, Cl, Br, SCN, SH). The compounds, whose substituting groups R and X are the same but the types of M are different, were separated satisfactorily by using the phosphates and decane-tributyl phosphate (1:1,1:2) as developing agents and showed the reference values in the order RfTi>RfZr>RfHf. Good separating capacity and the reference values in the order RfF>RfBr>Rfcl were also observed for the compounds with the same R and M But the different X. For the good separation of the compounds consisting of M=Ti, X=C1, SCN or Cl, SH and the same R, only the phosphate esters were found to be suitable as developing agents. As to the compounds consisting of M=Ti, Zr, Hf, X=C1, SCN and the same R, the complexing developing agents decane-acetone-phosphates esters (15:10:1) were suitable for the good separation. In considering of the insoluble or slightly soluble behavior of the samples in alkane, the considerable amount of diluent agent alkane was involved in the phosphates to decrease the polarity of the developing agent. It was found that as the diluent amount increased, the separating capacity was improved, with the results of the decrease of the Rf values.

【基金】 中国科学院科学基金
  • 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,1987年02期
  • 【下载频次】37
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