Novel synthesis and characterisation of ruthenium tris (4-methyl-4′-vinyl-2,2′-bipyridine) complexes
作者:Claire E Williams、Roy B Lowry、Jim Braven、Simon T Belt
DOI:10.1016/s0020-1693(01)00303-6
日期:2001.4
Abstract The synthesis of the ligand 4-methyl-4′-vinyl-2,2′-bipyridine is discussed. Methods previously reported presented problems in terms of yield and purity of a precursor. Traces of starting material (4,4′-dimethyl-2,2′-bipyridine) contaminated the product and this contaminant carried through to the synthesis of 4-methyl-4′-vinyl-2,2′-bipyridine. Thus, upon complexation to form ruthenium tris (4-methyl-4′-vinyl-2
摘要讨论了配体4-甲基-4'-乙烯基-2,2'-联吡啶的合成。先前报道的方法在前体的产率和纯度方面存在问题。痕量的起始原料(4,4'-二甲基-2,2'-联吡啶)污染了产物,该污染物被带入4-甲基-4'-乙烯基-2,2'-联吡啶的合成中。因此,在络合形成三(4-甲基-4'-乙烯基-2,2'-联吡啶)钌双(六氟磷酸盐)时,也存在双,单和非乙烯基络合物。钌三(4-甲基-4'-乙烯基-2,2'-联吡啶)双(六氟磷酸酯)的电聚合以产生高质量的聚合物薄膜需要每个配合物分子最大数量的乙烯基配体。混合物中配合物的相对百分比可以使用质子NMR来计算。该方法基于三和双化合物的乙烯基共振的积分值。然而,已经开发了一种简单的数学模型,其可以通过考虑4-甲基-4'-乙烯基-2,2'-联吡啶的纯度来预测络合之前混合物的组成百分比。4-(2-羟丙基)-4'-甲基-2,2'-联吡啶,4-甲基-4'-(E-丙-2-烯基)-2