一种钯配体化合物的合成

以2-萘胺为原料在氯化铜的作用下经过氧化偶联重排,得到1,1′-联萘-2,2′-二胺,然后依次经过重氮化、溴代和甲基化,得到2′-溴-2-N,N-二甲基-1,1′-联萘胺,收率49.7%。该联萘化合物在正丁基锂作用下,与二叔丁基氯化膦反应,得到最终的目标化合物,收率66.9%。4步反应的总收率33.3%。

ICP-OES测定双齿膦配体钯类化合物的含量

180℃条件下,于聚四氟乙烯消解罐加压消解双齿膦配体钯类化合物样品,研究了电感耦合等离子体发射光谱法(ICP-OES)测定双齿膦配体钯类化合物中钯含量的方法。采用ICP-OES法测定四种双齿膦配体钯类化合物样品,钯的检测值和理论值相近,结果准确,该检测法简便、快速,表明该检测法适合双齿膦配体钯类化合物中钯含量的测定。

Ionic palladium complex as an efficient and recyclable catalyst for the carbonylative Sonogashira reaction

The neutral palladium（Ⅱ） complex bis-[1-（5＇-diphenylphosphinothiazol-2＇-yl）-imidazolyl]dichloropalladium（Ⅱ）（1A） ligated by thiazolylimidazolyl-based phosphine（L1） in which thiazolylimidazolyl acted as an S- and N-donor provider with weak coordinating nature,and the ionic complex bis-[1-（5＇-diphenylphosphinothiazol-2＇-yl）-3-methylimidazolium]dichloropalladium（Ⅱ） trifluoromethanesulfonate（2A） ligated by thiazolylimidazolium-based phosphine（L2） after quaternization of L1 using methyl trifluoromethanesulphonate were synthesized.It was found that the introduced positive charges and strong electron-withdrawing effect in 2A not only led to changes in the configuration and structural stability of the complex,but also lowered its catalytic performance in carbonylative Sonogashira reactions.These effects reveal the important role of the N-donor in 1A.In addition,as an ionic palladium complex,2A combined with the room-temperature ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate could be recycled eight times as the catalyst in carbonylative Sonogashira reactions without detectable metal leaching.