SYNTHESIS AND PREPARATIVE HPLC-SEPARATION OF HETERONUCLEAR OLIGOMETALLOCENES - ISOLATION OF CATIONS OF RHODOCENYLFERROCENE, 1,1'-DIRHODOCENYLFERROCENE, AND 1-COBALTOCENYLFERROCENE,1'-RHODOCENYLFERROCENE

被引:11
作者
ANDRE, M
SCHOTTENBERGER, H
TESSADRI, R
INGRAM, G
JAITNER, P
SCHWARZHANS, KE
机构
[1] UNIV INNSBRUCK,INST ANORGAN & ANALYT CHEM,INNRAIN 52A,A-6020 INNSBRUCK,AUSTRIA
[2] BIOCHEM GMBH,A-6250 KUNDL,AUSTRIA
[3] UNIV INNSBRUCK,INST MINERAL & PETROG,A-6020 INNSBRUCK,AUSTRIA
关键词
PREPARATIVE COLUMN LIQUID CHROMATOGRAPHY; METALLOCENE SALT ISOLATION; HETERONUCLEAR TERMETALLOCENES;
D O I
10.1007/BF02269802
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
New members of mixed metal termetallocenes, 1,1'-dirhodoceniumylferrocene II, and 1-cobaltoceniumyl-,1'-rhodoceniumylferrocene III, were prepared by statistical nucleophilic attack of dilithioferrocene on equimolar amounts of cobaltocenium and rhodocenium hexafluorophosphate. Subsequent hydride abstraction with tritylium hexafluorophosphate yielded the respective termetallocene dications. Also a new bimetallocene monocation, ferrocenylrhodocenium I, a byproduct formed form partial protonation of dilithioferrocene, was identified. The new compounds were separated from undesired metallocenes, starting metallocenes, and byproducts by means of preparative HPLC. A reversed phase system was established which is sufficiently tuneable in selectivity to separate the different metallocene cationic species. The isolated compounds were characterized by NMR, IR, and ICP.
引用
收藏
页码:543 / 545
页数:3
相关论文
共 19 条
[1]  
ANGELICI RJ, 1963, J AM CHEM SOC, V85, P8733
[2]  
BAGHURST DR, 1989, J ORGANOMET CHEM, V368, P45
[3]  
BOSE R, 1990, ANGEW CHEM, V102, P589
[4]  
BRAUER G, 1981, HDB PRAPARATIVEN ANO, V3, P1849
[5]   THE STRUCTURE OF THE 3-2 ADDUCT OF 1,1'-DILITHIOFERROCENE WITH TETRAMETHYLETHYLENEDIAMINE [J].
BUTLER, IR ;
CULLEN, WR ;
NI, J ;
RETTIG, SJ .
ORGANOMETALLICS, 1985, 4 (12) :2196-2201
[7]   UBER AROMATENKOMPLEXE VON METALLEN .28. CYCLOPENTADIENYL-RHODIUM(I)-CYCLOPENTADIEN UND CYCLOPENTADIENYL-IRIDIUM(I)-CYCLOPENTADIEN [J].
FISCHER, EO ;
ZAHN, U .
CHEMISCHE BERICHTE-RECUEIL, 1959, 92 (07) :1624-1628
[8]  
GIEREN A, 1986, 1986 C M GERM AUSTR, P78
[9]  
INGRAM G, 1990, Z NATURFORSCH, pB45
[10]  
INGRAM G, UNPUB XRAY CRYSTAL S