高等学校化学学报

高等学校化学学报 ›› 1998, Vol. 19 ›› Issue (9): 1397.

• 论文 • 上一篇    下一篇

高效液相色谱直接分离μ-FcCCHCoW(CO)5(CpCOOC2H5)簇合物对映体

吴树林, 周志强, 丁二润, 殷元骐   

  1. 中国科学院兰州化学物理研究所, 羰基合成与选择氧化国家重点实验室, 兰州, 730000
  • 收稿日期:1997-12-09 出版日期:1998-09-24 发布日期:1998-09-24
  • 通讯作者: 殷元骐
  • 作者简介:吴树林,男,36岁,博士研究生.
  • 基金资助:

    中国科学院兰州化学物理研究所所长基金资助课题.

Direct Enantiomeric Resolution of Racemic μ-FcC-CHCoW-(CO)5(CpCOOC2H5) Using Amylopectin Tris(phenylcarbamate) Chiral Stationary by HPLC

WU Shu-Lin, ZHOU Zhi-Qiang, DING Er-Run, YIN Yuan-Qi   

  1. State key Laboratory of Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou, 730000
  • Received:1997-12-09 Online:1998-09-24 Published:1998-09-24

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摘要： 将三(苯基氨基甲酸)支链淀粉酯涂敷在硅胶上制成了手性固定相.将支链淀粉与过量的苯异氰酸酯在吡啶中反应得到的苯基氨基甲酸酯溶解并涂敷在用3-氨基丙基三乙氧基硅烷处理过的硅胶上,涂敷量为O.45／2.55(重量比).用此手性固定相拆分了外消旋的簇合物μ-FcC≡CHCoW(CO)5(CpCOOC2H5).拆分在室温下进行,洗脱液为甲醇,流速为O.5mL／min.

关键词: 高效液相色谱, 三(苯基氨基甲酸)支链淀粉酯, 外消旋双核簇合物

Abstract: Amylopectin tris(phenylcarbamate) was synthesized and used as the chiral stationary phase upon adsorbed over silica gel. For this purpose, amylopectin was allowed to react with an excess of phenylisocyanate in pyridine for 48 h. The carbamate was dissolved and adsorbed on silica gel which had been treated with 3-aminopropyltriethoxysilane. The weight ratio of the carbamate to the silica gel was 0.45:2.55. The racemic μ-FcC-CHCoW(CO)5 (CpCOOC2H5) prepared from μ-FcC-CHCo2.(CO)6 and (C2H5OOCCp)W(CO)3Na was resolved on this chiral stationary phase. Separation was carried out at room temperature, and methanol was used as the eluent at a flow rate of 0.5 mL/min.

Key words: HPLC, Amylopectin tris(phenylcarbamate), Dinuclear cluster

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