Publikation:

ansa-vanadocene complexes : syntheses, structures and ligand exchange reactions

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1997

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Dorer, Birgit
Prosenc, Marc-Heinrich
Rief, Ursula

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Collection of Czechoslovak Chemical Communications. 1997, 62(2), pp. 265-278. ISSN 0010-0765. eISSN 1212-6950. Available under: doi: 10.1135/cccc19970265

Zusammenfassung

Tetramethylethano-bridged vanadocene dichlorides (CH3)4C2(3-R-C5H3)2VCl2 with R = H, Me, t-Bu are obtained by reacting the corresponding ligand MgCl salts with vanadium(III) acetylacetonato compounds, followed by oxidation with PCl3 or AgCl. Smooth ligand exchange reactions of these ansa-vanadocene dichlorides afford acetylacetonato cations and binaphtholate complexes; from these, the dichlorides are regenerated by exposure to MgCl2 in THF solution. Separation of meso and rac isomers (as well as enantiomer separation) is achieved via corresponding binaphtholate complexes; conversion to the vanadium(III) diisonitrile cations (CH3)4C2(3-R-C5H3)2V(CNt-Bu)2+ allows an assessment of diastereoisomer ratios by 1H NMR. Lewis-acidic bistriflate derivatives of these ansa-vanadocene complexes are obtained from the dichlorides by reaction with silver triflate.

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540 Chemie

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ansa-metallocenes, vanadium, acetylacetonato complex, chiral, enantioseparation

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ISO 690DORER, Birgit, Marc-Heinrich PROSENC, Ursula RIEF, Hans-Herbert BRINTZINGER, 1997. ansa-vanadocene complexes : syntheses, structures and ligand exchange reactions. In: Collection of Czechoslovak Chemical Communications. 1997, 62(2), pp. 265-278. ISSN 0010-0765. eISSN 1212-6950. Available under: doi: 10.1135/cccc19970265
BibTex
@article{Dorer1997ansav-23757,
  year={1997},
  doi={10.1135/cccc19970265},
  title={ansa-vanadocene complexes : syntheses, structures and ligand exchange reactions},
  number={2},
  volume={62},
  issn={0010-0765},
  journal={Collection of Czechoslovak Chemical Communications},
  pages={265--278},
  author={Dorer, Birgit and Prosenc, Marc-Heinrich and Rief, Ursula and Brintzinger, Hans-Herbert}
}
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    <dcterms:abstract xml:lang="eng">Tetramethylethano-bridged vanadocene dichlorides (CH&lt;sub&gt;3&lt;/sub&gt;)&lt;sub&gt;4&lt;/sub&gt;C&lt;sub&gt;2&lt;/sub&gt;(3-R-C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;3&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;VCl&lt;sub&gt;2&lt;/sub&gt; with R = H, Me, t-Bu are obtained by reacting the corresponding ligand MgCl salts with vanadium(III) acetylacetonato compounds, followed by oxidation with PCl&lt;sub&gt;3&lt;/sub&gt; or AgCl. Smooth ligand exchange reactions of these ansa-vanadocene dichlorides afford acetylacetonato cations and binaphtholate complexes; from these, the dichlorides are regenerated by exposure to MgCl&lt;sub&gt;2&lt;/sub&gt; in THF solution. Separation of meso and rac isomers (as well as enantiomer separation) is achieved via corresponding binaphtholate complexes; conversion to the vanadium(III) diisonitrile cations (CH&lt;sub&gt;3&lt;/sub&gt;)&lt;sub&gt;4&lt;/sub&gt;C&lt;sub&gt;2&lt;/sub&gt;(3-R-C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;3&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;V(CNt-Bu)&lt;sub&gt;2&lt;/sub&gt;&lt;sup&gt;+&lt;/sup&gt; allows an assessment of diastereoisomer ratios by &lt;sup&gt;1&lt;/sup&gt;H NMR. Lewis-acidic bistriflate derivatives of these ansa-vanadocene complexes are obtained from the dichlorides by reaction with silver triflate.</dcterms:abstract>
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