辛酸铑(Ⅱ)的合成及其结构表征

Synthesis and Structure of Rhodium Octanoate

以三氯化铑为原料,在弱酸性条件下,直接与辛酸回流反应,成功制备了辛酸铑(II),产率>95%,产品纯度>99.0%,适合工业化生产要求。辛酸铑(II)样品通过质谱分析、红外光谱分析和单晶X射线衍射分析确定为二聚体,以羧基为桥联配体,形成灯笼状的空间立体结构。

A new method was established to synthesize rhodium octanoate, an important catalyst for C - H insertion process. The direct reaction between RhCl3 · 3H2O and CTH15COOH in water at pH-≈5 pro- duced rhodium octanoate with a yield of more than 95% based on RhCl3 · 3H2O. The purity of the prod- uct was determined by HPLC to be greater than 99.0%. The structural studies by MS, IR, NMR and sin- gle X - ray diffraction reveal that rhodium octanoate is a dimeric coordination compound in which two rho- dium atoms are bridged by four octanoate COO - groups, forming ＇ lantern - like＇ structure.