Facultatea de Chimie si Inginerie Chimica, Universitatea Babes-Bolyai, RO-400028, Cluj-Napoca, Romania.
Dalton Trans. 2010 Jul 28;39(28):6410-8. doi: 10.1039/c003318a. Epub 2010 May 10.
Hypervalent organoantimony(III) compounds of the type [2-(Me2NCH2)C6H4]PhSbCl (1), [2-(Me2NCH2)C6H4]MesSbBr (7) and [2-(Me2NCH2)C6H4]nAr(3-n)Sb [n = 1, Ar = Ph (4), Mes (9); n = 2, Ar = Ph (5), Mes (10)] were prepared via salt elimination reactions between [2-(Me2NCH2)C6H4]Li and MesMgBr and PhnSbCl(3-n), [2-(Me2NCH2)C6H4]SbBr2 or [2-(Me2NCH2)C6H4]nSbCl(3-n) (n = 1, 2), in appropriate molar ratios. Halogen exchange reactions with aqueous KBr or KI gave [2-(Me2NCH2)C6H4]ArSbX [Ar = Ph, X = Br (2), I (3); Ar = Mes, X = I (8)]. Metathesis reaction between 1 and MesMgBr affords [2-(Me2NCH2)C6H4]PhMesSb (6). Compounds 1-10 were investigated by means of NMR (1H, 13C) in solution and by mass spectrometry. The investigation of the molecular structures of 2-8 by single-crystal X-ray diffraction revealed that the nitrogen atoms of the pendant CH2NMe2 arms are strongly coordinated to the antimony atoms. All compounds exhibit chirality and crystallize as racemic mixtures.
高荷电价的有机锑(III)化合物[2-(Me2NCH2)C6H4]PhSbCl(1)、[2-(Me2NCH2)C6H4]MesSbBr(7)和[2-(Me2NCH2)C6H4]nAr(3-n)Sb[n=1,Ar=Ph(4),Mes(9);n=2,Ar=Ph(5),Mes(10)]是通过[2-(Me2NCH2)C6H4]Li与MesMgBr和PhnSbCl(3-n)、[2-(Me2NCH2)C6H4]SbBr2或[2-(Me2NCH2)C6H4]nSbCl(3-n)(n=1,2)之间的盐消除反应制备的，其摩尔比适当。与水合 KBr 或 KI 的卤素交换反应得到[2-(Me2NCH2)C6H4]ArSbX[Ar=Ph,X=Br(2),I(3);Ar=Mes,X=I(8)]。1 与 MesMgBr 之间的复分解反应得到[2-(Me2NCH2)C6H4]PhMesSb(6)。通过 NMR(1H,13C)在溶液中和质谱研究了化合物 1-10。通过单晶 X 射线衍射研究了 2-8 的分子结构，发现悬垂的 CH2NMe2 臂的氮原子与锑原子强烈配位。所有化合物都表现出手性，结晶为外消旋混合物。
