| Article ID | Journal | Published Year | Pages | File Type |
|---|---|---|---|---|
| 1307793 | Inorganica Chimica Acta | 2006 | 12 Pages |
Ferrocene reacts with hexafluoroacetone trihydrate in refluxing octane to afford >80% yields of [CpFe(η5-C5H4C(CF3)2OH)] (X-ray), carrying out the reactions at 180 °C gives an additional 5% yield of [Fe(η5-C5H4C(CF3)2OH)2] (X-ray).The mono alcohol is lithiated with ButOK/BunLi/TMEDA affording partial conversion to mixtures of [CpFe(1,2-η5-C5H3C(CF3)2OH)(X)] and [Fe(η5-C5H4X)(1,2-η5-C5H3C(CF3)2OH)(X)] (X = SMe, CPh2OH) upon reaction with Me2S2 or OCPh2.For X = CPh2OH both structures are crystallographically characterised.Enantiopure [CpFe(1,2-η5-C5H3C(CF3)2OH)(SMe)] can be prepared from (R)-[CpFe(η5-C5H4S(O)C6H4Me)] via [CpFe(1,2-η5-C5H3S(O)C6H4Me)(C(CF3)2OH)] (X-ray) or [CpFe(1,2-η5-C5H3S(O)C6H4Me)(SMe)].Related procedures allow the preparation of [CpFe(1,2-η5-C5H3CPh2OH)(Y)] (Y = SMe, CHO (X-ray), C(CF3)2OH) and[CpFe(1,2-η5-C5H3C(CF3)2OH)(CHO)].
Graphical abstractThe preparation of new ligand structures based on [CpFe(η5-C5H3(C(CF3)2OH)(E))] (E = SMe, CPh2OH, CHO). These are attained either by directed lithiation of [CpFe(η5-C5H4(C(CF3)2OH))] which results in the formation of the desired species and a [Fe(η5-C5H3(C(CF3)2OH(E)))(η5-C5H4E)] (E = SMe, CPh2OH) co-product or by sequential lithiation/trap reactions of [CpFe(η5-C5H4(S(O)4-Tol))].Crystal structures of examples of these complexes are presented.Figure optionsDownload full-size imageDownload as PowerPoint slide
