Department of Chemistry, National Changhua University of Education, Changhua, Taiwan 500.
Inorg Chem. 2010 Jan 4;49(1):136-43. doi: 10.1021/ic9016189.
The new pyrrolyl-linked pincer-type ligand, [C(4)H(2)NH(2-CH(2)NH(t)Bu)(5-CH(2)NMe(2))] (1), that has been employed conveniently in high yield by treatment of (2-t-butylaminomethyl)pyrrole with 1 equiv of formaldehyde and dimethylamine hydrochloride each in diethylether and its corresponding aluminum derivative, [C(4)H(2)N(2-CH(2)NH(t)Bu)(5-CH(2)NMe(2))]AlH(2) (2), that has been generated from Me(3)N.AlH(3) using diethylether as a solvent are described. Furthermore, reactions of 2 with 2 equiv of either 1,3-diphenylpropane-1,3-dione in diethylether or phenyl thioisocyanate in dichloromethane interestingly formed [C(4)H(2)N(2-CH(2)NH(t)Bu)(5-CH(2)NMe(2))]Al(PhCOCHCOPh)(2) (3) and [C(4)H(2)N(2-CH(2)NH(t)Bu)(5-CH(2)NMe(2))]Al(SCHNPh)(2) (4), respectively, following deprotonation or hydroalumination reaction kinetics under a dry nitrogen environment. All of the compounds have been subjected to the X-ray diffraction technique in the solid state as well as characterized by NMR spectra.
新型吡咯基连接的钳子型配体[C(4)H(2)NH(2-CH(2)NH(t)Bu)(5-CH(2)NMe(2))](1),可通过(2-叔丁氨基甲基)吡咯与等摩尔的甲醛和二甲胺盐酸盐在二乙醚中的反应方便地以高产率获得,其相应的铝衍生物[C(4)H(2)N(2-CH(2)NH(t)Bu)(5-CH(2)NMe(2))]AlH(2)(2),可通过 Me(3)N.AlH(3)在二乙醚中作为溶剂生成。此外,2 与 2 当量的 1,3-二苯基丙烷-1,3-二酮在二乙醚或苯硫异氰酸酯在二氯甲烷中的反应有趣地形成了[C(4)H(2)N(2-CH(2)NH(t)Bu)(5-CH(2)NMe(2))]Al(PhCOCHCOPh)(2)(3)和[C(4)H(2)N(2-CH(2)NH(t)Bu)(5-CH(2)NMe(2))]Al(SCHNPh)(2)(4),分别在干燥氮气环境下进行脱质子或氢铝化反应动力学。所有化合物均在固态下通过 X 射线衍射技术进行了表征,并通过 NMR 谱进行了表征。