Exploring Alternative Synthetic Routes for the Preparation of Five-Coordinate Diamidoamine Group 4 Metal Complexes
作者:Alicia R. Morgan、Michael Kloskowski、Felix Kalischewski、Aaron H. Phillips、Jeffrey L. Petersen
DOI:10.1021/om0580349
日期:2005.10.1
Efficient synthetic routes for the preparation of electrophilic titanium and zirconium complexes featuring a tridentate diamidoamine ligand have been developed. The five-coordinate titanium dichloride complexes [(MesNCH2CH2)2NR]TiCl2 (R = H (3), SiMe3 (4)) are conveniently prepared from the amine elimination reactions of the triamines (MesNHCH2CH2)2NR (R = H (1), SiMe3 (2)) with Ti(NEt2)2Cl2. Treatment
已经开发了制备具有三齿二氨基胺配体的亲电钛和锆配合物的有效合成途径。由三胺(MesNHCH 2 CH 2)的胺消除反应可方便地制备五配位二氯化钛配合物[(MesNCH 2 CH 2)2 NR] TiCl 2(R = H(3),SiMe 3(4))。2 NR(R = H(1),SiMe 3(2))与Ti(NEt 2)2 Cl 2。Ti(NEt 2的处理)4当量为2当量的SiMe 3 Cl提供了一种制备Ti(NEt 2)2 Cl 2的有效方法。通过Zr(苄基)2 Cl 2(Et )的甲苯消除反应合成相应的五坐标锆同系物[(MesNCH 2 CH 2)2 NR] ZrCl 2(R = H(5),SiMe 3(6))。2 O)2分别具有1和2。热不稳定且光敏的Zr(苄基)2Cl 2(Et 2 O)2物种可以从Zr(苄基)4与2当量的[NEt 3 H] Cl在乙醚中,在黑暗中于0°C的反应原位制备。