Efficient synthesis of the cyclometalated complex fac-[Rh(ppy)3] (ppy=2-phenylpyridinato)

被引：13
|
作者：
Boettcher, Hans-Christian [1 ]
Graf, Marion [1 ]
Suenkel, Karlheinz [1 ]
Krueger, Hartmut [2 ]
机构：
[1] Univ Munich, Dept Chem, D-81377 Munich, Germany
[2] Fraunhofer Inst Angew Polymerforsch, D-14476 Potsdam, Germany
来源：
INORGANICA CHIMICA ACTA | 2011年 / 370卷 / 01期
关键词：
Rhodium; Olefinic complexes; Oxidative addition; Cyclometalated complexes; IRIDIUM(III); RHODIUM(III);
D O I：
10.1016/j.ica.2011.01.041
中图分类号：
O61 [无机化学];
学科分类号：
070301 ; 081704 ;
摘要：
A new convenient high-yield synthesis of the tris-cyclometalated complexes fac-[Rh(ppy)(3)] (4; ppy = 2-phenylpyridinato) was developed. Complex 4 was prepared in a kind of one-pot synthesis starting from in situ prepared [Rh(acac)(coe)(2)] (2) which was heated in refluxing 2-phenylpyridine for a short time. After purification by filtration over alumina, compound 4 was obtained in yields of 65%. Also [Rh(a-cac)(ppy)(2)] (3) was prepared in a similar manner by oxidative addition of Hppy in refluxing toluene in high yields. In contrast to previous findings with the analogous iridium compounds, there was not any hint at the formation of the isomer mer-[Rh(ppy)(3)] using similar reaction conditions as applied for iridium. Furthermore the compound [{Rh(mu-Cl)(ppy)(2)}(2)] (5) was prepared from [{Rh(mu-Cl)(coe)(2)}(2)] (1) and Hppy in refluxing toluene in nearly quantitative yield. (C) 2011 Elsevier B.V. All rights reserved.
引用
收藏
页码：523 / 525
页数：3
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