当前位置: X-MOL 学术J. Organomet. Chem. › 论文详情
Our official English website, www.x-mol.net, welcomes your feedback! (Note: you will need to create a separate account there.)
Quinoxaline-anellated N,N´-dialkylimidazolium salts and iPr2quinox-NHC-Pd halide complexes
Journal of Organometallic Chemistry ( IF 2.1 ) Pub Date : 2020-08-26 , DOI: 10.1016/j.jorganchem.2020.121487
Saravanakumar Shanmuganathan , Carola Schulzke , Peter G. Jones , Joachim W. Heinicke

Excess isopropyl- or neopentylamine react with dichloroquinoxaline to the respective diaminoquinoxalines and further with triethyl orthoformate to quinoxaline-anellated imidazolium salts as precursors for quinoxaline-anellated imidazolin-2-ylidene transition metal complexes. The bulky tert-butylamine replaces only one chlorine atom and opens, via a second amination step, a route to unsymmetrically N,N´-substituted diaminoquinoxalines as potential precursors to quinox-NHCs with different N,N´-substituents. A convenient high-yield access to the new trans-(iPr2quinoxImy)2PdX2 (X = Cl, I) complexes, supplementing an earlier communication on the first quinox-NHC-Rh(COD)Cl and Ag complexes, was provided by the reaction of PdCl2/NaOAc or Pd(OAc)2/2KI with iPr2quinoxImyH+ PF6 via deprotonation of the C-H acidic precursor salt with acetate. The compounds were characterized by NMR data, assigned via 2D and proton-coupled 13C NMR spectra, and/or crystal structure analyses. Short CMe2-H···Pd and Pd-Cl···CII distances suggest weak stabilizing interactions, in solution indicated by unusually strong downfield shifts of the CMe2H protons.



中文翻译:

喹喔啉修饰的N,N′-二烷基咪唑鎓盐和i Pr 2喹喔啉-NHC-Pd卤化物配合物

过量的异丙基或新戊胺与二氯喹喔啉反应成相应的二氨基喹喔啉,并进一步与原甲酸三乙酯反应成喹喔啉修饰的咪唑啉盐,作为喹喔啉修饰的咪唑啉-2-亚烷基过渡金属配合物的前体。庞大的丁胺仅取代一个氯原子,并通过第二步胺化步骤,开辟了一条路线,使不对称的N,N'-取代的二氨基喹喔啉成为具有不同N,N'-取代基的喹喔啉-NHC的潜在前体。方便获得新反式-(i Pr 2 quinoxImy)2 PdX 2的高产率(X = Cl,I)配合物,通过PdCl 2 / NaOAc或Pd(OAc)2 / 2KI与i Pr的反应提供了对第一种喹喔啉-NHC-Rh(COD)Cl和Ag配合物的早期通讯的补充。2 quinoxImyH + PF 6 -经由与醋酸CH酸性前体盐的去质子化。化合物通过NMR数据(通过2D和质子耦合的13 C NMR光谱分配)和/或晶体结构分析进行表征。CMe 2 -H···Pd和Pd-Cl····C II距离短,表明在溶液中CMe 2 H的异常强下移表明稳定作用弱 质子

更新日期:2020-09-08
down
wechat
bug