Ruthenium macrocycles bearing pyridine bis(carboxamide): synthesis, structure, and catalytic activity for hydrosilylation
Ruthenium macrocycles bearing pyridine bis(carboxamide): synthesis, structure, and catalytic activity for hydrosilylation
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带有吡啶双（甲酰胺）的钌大环：合成、结构和氢化硅烷化的催化活性
DOI：
10.1039/d0nj06133f
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发表时间：
2021
影响因子：
3.3
通讯作者：
Takata Toshikazu
中科院分区：
文献类型：
--
作者：
Sato Hiroki;Tsukamoto Tadashi;Sogawa Hiromitsu;Kuwata Shigeki;Takata Toshikazu
合成并表征了一个钳形大环配体MC 33与Ru（MC 33）（CO）n（L）2−n（L = H2O，PPh 3，P（OEt）3; n = 1，2）的配合物。采用含双甲酰胺结构的钳形配体和钌（0）羰基前体合成了Ru（MC 33）（CO）2（H2O），产率高达97%。另外，与Ru（MC 33）（CO）2（H2O）同样地，合成了具有钳型非环状配体AC的Ru（AC）（CO）2（H2O）。通过CO与磷配体的选择性热配体交换，形成单（膦）和双（亚磷酸酯）配合物。配合物的结构进行了研究，通过核磁共振光谱，红外光谱，电喷雾电离高分辨质谱，和X-射线分析。此外，它们对硅氢加成反应的催化活性也得到了证实。
Ruthenium complexes Ru(MC33)(CO)n(L)2−n (L = H2O, PPh3, P(OEt)3; n = 1, 2) with a pincer-type macrocyclic ligand MC33 with a cavity were synthesized and characterized. Ru(MC33)(CO)2(H2O) was obtained in yields of up to 97% using a pincer-type ligand containing the bis(carboxamide) moiety and ruthenium(0) carbonyl precursor. Ru(AC)(CO)2(H2O) having a pincer-type acyclic ligand AC was also synthesized in a similar manner to Ru(MC33)(CO)2(H2O). Mono(phosphine) and bis(phosphite) complexes were formed via the selective thermal ligand exchange of CO with phosphorus ligands. The structure of the complexes was studied by nuclear magnetic resonance spectroscopy, infrared spectroscopy, electrospray ionization–high-resolution mass spectroscopy, and X-ray analyses. In addition, their catalytic activity for hydrosilylation was demonstrated.