Schoeps Dirk, Buhr Kristian, Dijkstra Marga, Ebert Katrin, Plenio Herbert
Anorganische Chemie im Zintl-Institut, Petersenstr. 18, Technische Universität Darmstadt, 64287 Darmstadt, Germany.
Chemistry. 2009;15(12):2960-5. doi: 10.1002/chem.200802153.
A mass-tagged N-mesityl imidazolinium salt with four additional -CH(2)NCy(2) substituents was synthesized, leading to a molecular mass of nearly 1100 g mol(-1) in the corresponding carbene ligand. This mass-tagged ligand was used to generate the respective Grubbs II and Grubbs-Hoveyda type complexes. The catalytic activity of the latter complex was tested in several olefin metathesis reactions and found to be slightly superior to that of the related N-mesityl based complex. In batchwise solvent resistant nanofiltration experiments the ruthenium complex dissolved in toluene and following a metathesis reactions was efficiently retained (>99.8 %) by a single nanofiltration; the permeate contained less than 4 ppm of Ru. Equally efficient catalyst retention was observed in a membrane reactor utilized for the continuous synthesis of a RCM product.
合成了一种带有四个额外-CH(2)NCy(2)取代基的质量标记的N-均三甲苯基咪唑啉鎓盐,使得相应卡宾配体的分子量接近1100 g mol(-1)。该质量标记的配体用于生成各自的格拉布催化剂II型和格拉布-霍维达型配合物。在几个烯烃复分解反应中测试了后一种配合物的催化活性,发现其略优于相关的基于N-均三甲苯基的配合物。在间歇式耐溶剂纳滤实验中,溶解在甲苯中的钌配合物在复分解反应后通过单次纳滤被有效截留(>99.8%);渗透物中Ru含量低于4 ppm。在用于连续合成RCM产物的膜反应器中也观察到了同样高效的催化剂截留效果。