微波辅助合成芳烃钌（Ⅱ）配合物[（η^6-C6H5）Ru（PIP）Cl]Cl·2H2O  

Microwave-assisted synthesis of arene Ru（Ⅱ） complex [（η^6-C6H5）Ru（PIP）Cl]Cl·2H2O

作　　者：陈艾纯[1] 吴琼[1] 陈燕华[1] 梅文杰[1] 吴韦黎[1] 胡晓莹[1] 吴剑[1] 汪保国[2] 

机构地区：[1]广东药学院药科学院,广东广州510006 [2]广东药学院公共卫生学院,广东广州510310

出　　处：《广东药学院学报》2013年第1期21-24,共4页Academic Journal of Guangdong College of Pharmacy

基　　金：广州市科技计划项目(2011J5200017);广州市中小企业创新基金;广东药学院中青年骨干教师培养基金;广东药学院创新实验项目

摘　　要：目的探讨应用微波辅助合成技术制备芳烃钌(Ⅱ)化合物[(η6-C6H6)Ru(PIP)Cl]Cl.2H2O(3)。方法首先以RuCl3.nH2O、1,3-环己二烯和1,10-邻菲啰啉为原料微波辐射下制备得到芳烃钌前体[(η6-C6H6)RuCl2]2(1)和2-苯基-咪唑并[4,5f][1,10]菲啰啉(PIP,2),然后,在二氯甲烷溶液中,微波辐射1与2制备芳烃钌(Ⅱ)配合物3;采用ESI-MS、IR、1H-NMR、13C-NMR对目标配合物进行表征。结果 60℃条件下,化合物1与2在二氯甲烷溶液微波辐射30 min,制备得到了芳烃钌配合物3,反应产率为90.3%;目标产物经ESI-MS、IR、1H-NMR和13C-NMR表征,实验值与理论值基本一致。结论与传统加热方法相比,微波辅助合成芳烃钌配合物明显缩短了反应时间,提高了反应产率。Objective To research the preparation of arene Ru（Ⅱ） complex [（η6-C6H6）Ru（PIP）Cl]Cl·2H2O（3） by using microwave-assisted synthesis technology.Methods [（η6-C6H6）RuCl2]2（1） was synthesized from RuCl3·nH2O and 1,3-cyclohexadiene by using microwave-assisted synthesis technology,and 2-phenyl-imidazolephenanthroline（PIP,2） also synthesized from 1,10-phenanthroline-5,6-dione and benzaldehyde under microwave irradiation,and then 2 and 3 were mixed in CH2Cl2 solution to prepare [（η6-C6H6）Ru（PIP）Cl]Cl·2H2O（3） under the irradiation microwave.The target complex 3 was characterized by using ESI-MS,IR,1H-NMR and 13C-NMR spectra.Results Arene Ru（Ⅱ） complex 3 was prepared from 1 and 2 in CH2Cl2 at 60℃ for 30 min under microwave irradiation with a yield of 90.3%,and characterized by ESI-MS,IR,1H-NMR and 13C-NMR spectra.Conclusion A novel arene ruthenium（Ⅱ） complexes 3 have been synthesized under the irradiation of microwave,and with far more less time and higher yield compared with the conventional method.

关 键 词：微波 2-苯基-咪唑并[4 5f][1 10]菲啰啉 芳烃钌(Ⅱ)配合物 

分 类 号：O641.4[理学—物理化学]