Attachment of Chelating Ligand Pockets to Tinorganyl Moieties

Attachment of Chelating Ligand Pockets to Tinorganyl Moieties
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DOI:
10.1002/ejic.201400089
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发表时间:
2014-05
影响因子:
2.3
通讯作者:
Beatrix E. K. Barth;K. Harms;S. Dehnen
Beatrix E. K. Barth;K. Harms;S. Dehnen
中科院分区:
化学3区
文献类型:
--
作者:
Beatrix E. K. Barth;K. Harms;S. Dehnen

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采用多种方法合成了一种新的含2,2 ′,6 ′,2 ″-三联吡啶结构的锡有机化合物。通过5步反应合成了Ph 3Sn(CH 2)3 OPhttpy [HOttpy = 2,6-bis(2′-pyridyl)-4′-(p-hydroxyphenyl)pyridine],总收率为51%。用氢碘酸卤代产生一种新的双核配合物阳离子,这是由两个一价阳离子头-尾配位的结果。此外,已经优化了已知中间体的合成和产率。通过119 Sn NMR、1H NMR、13 C NMR和ESI质谱以及单晶X-射线衍射对产物进行了分析和鉴定。
Several approaches have been undertaken to realize the synthesis of a new tinorganyl compound with a 2,2′,6′,2″-terpyridine moiety. A synthesis pathway consisting of five steps with an overall yield of 51 % was successful in producing Ph3Sn(CH2)3OPhttpy [HOttpy = 2,6-bis(2′-pyridyl)-4′-(p-hydroxyphenyl)pyridine], and insight has been gained into (partial) halogenation reactions with this unprecedented tinorganyl compound. Halogenation with hydroiodic acid produced a new dinuclear complex cation that resulted from head-to-tail coordination of two monocations. Furthermore, synthesis and yields of already known intermediates have been optimized. The products were analyzed and identified by 119Sn NMR, 1H NMR, and 13C NMR spectroscopy and ESI mass spectrometry, as well as by means of single-crystal X-ray diffraction.