在 N,N-二甲基甲酰胺介质中，将水合三氯化铑与乙酰丙酮加热回流，一步合成了乙酰丙酮·二羰基铑([Rh(CO)2(acac)]2)，产率为93%；以正丁烷为介质，[Rh(CO)2(acac)]2与三苯基磷(PPh3)定量反应，得到乙酰丙酮·三苯基膦·羰基铑(Rh(acac)(PPh3)(CO))，产率为99%。用气相扩散法和溶剂缓慢挥发法分别培养出[Rh(CO)2(acac)]2和 Rh(acac)(PPh3)(CO)单晶，元素分析的结果表明产物为目标化合物。用X射线单晶衍射仪对其结构进行了表征，获得了晶体结构参数，结果表明2种化合物均为三斜晶系、P-1空间群，[Rh(CO)2(acac)]2为二聚体化合物，Rh(acac)(PPh3)(CO)为单核配合物。
Rh(CO)2(acac)]2 was synthesized in one-step process from RhCl3·3H2O in DMF by adding acac as the anion ligand. The yield was 93%. A quantitative reaction between [Rh(CO)2(acac)]2 and PPh3 in n-butane gave rise to the formation of Rh(acac)(PPh3)(CO) with a yield of 99%. Single crystals of two complexes were prepared, respectively, via a gaseous diffusion method and a solvent evaporation technique, and were subjected to X-ray diffraction analysis. The results show both complexes are in the triclinic system with a space group of P-1. [Rh(CO)2(acac)]2 displays a dimmeric structure with Rh-Rh bond being 3.417 ?, whereas Rh(acac)(PPh3)(CO) has a normal mononuclear structure.
参考文献
| [1] | 王胜国;熊晓东;隋国荣;张英魁.乙酰丙酮三苯基膦羰基铑（Ⅰ）的合成与表征[J].贵金属,2005(1):43-46. |
| [2] | 李晨;蒋凌云;于海斌.乙酰丙酮二羰基铑（I）的制备合成[J].广州化工,2014(15):140-141. |
| [3] | 郇昌永;季来军;马磊.乙酰丙酮二羰基铑（Ⅰ）的合成与表征[J].广州化工,2012(3):77-78. |
| [4] | 何沛林;晏彩先;郑萍;常桥稳;刘伟平;谢笑天.双[2-（对甲苯基）吡啶]乙酰丙酮合铱的合成及结构表征[J].贵金属,2015(2):44-48. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%