Silva Rafaela A L, Vieira Bruno J C, Andrade Marta M, Santos Isabel C, Rabaça Sandra, Belo Dulce, Almeida Manuel
Centro de Ciências e Tecnologias Nucleares, Campus Tecnológico e Nuclear, Instituto Superior Técnico, Universidade de Lisboa, Estrada Nacional 10, ao km 139,7, 2695-066 Bobadela LRS, Portugal.
Beilstein J Org Chem. 2015 May 5;11:628-37. doi: 10.3762/bjoc.11.71. eCollection 2015.
Two new dithiolene ligand precursors, containing fused TTF and alkyl thiophenic moieties 3,3'-{[2-(5-(tert-butyl)thieno[2,3-d][1,3]dithiol-2-ylidene)-1,3-dithiole-4,5-diyl]bis[sulfanediyl]}dipropanenitrile (α-tbtdt, 1), and 3,3'-{[2-(5-methylthieno[2,3-d][1,3]dithiol-2-ylidene)-1,3-dithiole-4,5-diyl]bis[sulfanediyl]}dipropanenitrile (α-mtdt, 2), were synthesized and characterized. The electrochemical properties of these electronic donors were studied by cyclic voltammetry (CV) in dichloromethane. Both compounds show two quasi-reversible oxidation processes, versus Ag/AgCl, typical of TTF donors at E (1) 1/2 = 279 V and E (2) 1/2 = 680 V for 1 and E (1) 1/2 = 304 V and E (2) 1/2 = 716 V in the case of 2. The single-crystal X-ray structure of 1 and of a charge transfer salt of 2, (α-mtdt)[Au(mnt)2] (3), are reported.
合成并表征了两种新型二硫纶配体前体，它们含有稠合的四硫富瓦烯（TTF）和烷基噻吩部分，分别为3,3'-{[2-(5-(叔丁基)噻吩并[2,3-d][1,3]二硫醇-2-亚基)-1,3-二硫杂环戊烯-4,5-二基]双[亚磺酰基]}二丙腈（α-tbtdt，1）和3,3'-{[2-(5-甲基噻吩并[2,3-d][1,3]二硫醇-2-亚基)-1,3-二硫杂环戊烯-4,5-二基]双[亚磺酰基]}二丙腈（α-mtdt，2）。在二氯甲烷中通过循环伏安法（CV）研究了这些电子给体的电化学性质。两种化合物均显示出两个准可逆氧化过程，相对于Ag/AgCl，这是TTF给体的典型特征，对于1，E(1)1/2 = 279 V和E(2)1/2 = 680 V，对于2，E(1)1/2 = 304 V和E(2)1/2 = 716 V。报道了1的单晶X射线结构以及2的电荷转移盐(α-mtdt)[Au(mnt)2]（3）的单晶X射线结构。
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