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  • 1
    Electronic Resource
    Electronic Resource
    Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, LXI Das Verhalten von η2-Thiophosphinito-Komplexen des Cobalts gegenüber elektronenarmen Alkinen (1989)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 53-58 
    Details
    ISSN: 0009-2940
    Keywords: Cyclocotrimerization ; Furan derivatives ; η2-Thiophosphinito complexes of cobalt ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal-Containing Heterocycles: Preparation, Properties, Reaction, LXI. - The Behavior of η-Thiophosphinito Complexes of Cabalt towards Electron-Poor AlkynesIn the presence of PPh3, the (η2-thiophosphinito)cobalt complex Ph3P[cO](η-S=2)[Co] = Co(Co)2 reacts with the alkynes R′C≡CR′ (2a-d) [R′ = CO2R: R = Me (a), Et (b), iPr (c), Cy (d)] to give the thiaphosphacobaltacyclopentadienes . According to an X-ray structural analysis, 3b crystallizes in the space group P1 with Z = 2. In the planar five-membered ring cobalt has a trigonal bipyramidal geometry. The furan derivative 7a is obtained from 3a and 2a by hydrolytic decomposition of the nonisolable cyclotrimerisation product 6a. Furan 7a is formed also straightforwardly by the reaction of 1 with excess of 2a in the absence of PPh3. The reaction of 3b with the mixed substituted alkyne CH3C≡CCO2CH3 (2e) affords the isomeric furan derivatives 8 and 9.
    Notes: In Gegenwart von PPh3 setzt sich der (η2-Thiophosphinito)cobalt-Komplex Ph3P[cO](η-S=2)[Co] = Co(Co)2 mit den Alkinen R′C≡CR′ (2a-d) [R′ = CO2R: R = Me (a), Et (b), iPr (c), Cy (d)] zu den Thiaphosphacobaltacyclopentadienen Ph3 um. Nach einer Röntgenstrukturanalyse kristallisiert 3b in der Raumgruppe P1 mit Z = 2. In dem planaren Fünfring besitzt Cobalt eine trigonalbipyramidale Geometrie. Aus 3a und 2a erhält man über das nicht isolierbare Cyclotrimerisat 6a durch dessen hydrolytischen Abbau und Umlagerung das Furanderivat 7a, welches bei Abwesenheit von PPh3 auch direkt durch Reaktion von 1 mit überschüssigem 2a entsteht. Die Umsetzung von 3b mit dem gemischt substituierten Alkin CH3C≡CCO2CH3 (2e) liefert die isomeren Furanderivate 8 und 9.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19891220109
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  • 2
    Electronic Resource
    Electronic Resource
    Preparation, Properties, and Reactions of Metal-Containing Heterocycles, XCVPart XCIV: Ref.[1].. Transition-Metal-Mediated Cyclocotrimerization of Selenophosphinites with Activated AlkynesDedicated to Professor Rudolf Taube on the occasion of his 65th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 945-951 
    Details
    ISSN: 0009-2940
    Keywords: Cyclocotrimerization ; Selenophosphinites ; Alkynes, activated ; Selenophenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Selenophosphinito complexes (OC)4Mn(η2-Se\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}PR21) (2a, b) [R1 = cyc-Hex (a), tBu (b)] are formed by the reaction of BrMn(CO)5 with the phosphane selenides R21HPSe (1a, b) in the presence of the auxiliary base Et(iPr)2N. According to an X-ray structural analysis, 2a crystallizes in the space group \documentclass{article}\pagestyle{empty}\begin{document}$ P\bar 1 $\end{document} with Z = 2. The dimeric complex [(OC)4Mn(μ-Se\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}PMe2)]2 (4c) is not obtained in a straightforward way. Compound 4c is only obtained via the intermediate Br(OC)4Mn-Se\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}P(H)Me2 (3c) by HBr elimination with nBuLi. Complex 3c is formed by replacement of carbon monoxide in BrMn(CO)5 by Me2HPSe (1c). A dissociative equilibrium between [(OC)4 Mn(μ-Se\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}PMe2)]2 (4c) and the monomeric species (OC)4Mn(\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}2-Se\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}PMe2) was not observed. The cyclocotrimerization of the 〉P\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}Se function with the activated alkynes ZC≡CZ [Z = CO2R2; R2 = Me (d), Et (e), iPr (f), cyc-Hex (g)] was successful only in the case of the cyclohexyl derivative 2a to give the selenaphosphamanganabicycloheptadienes 5d - g. An X-ray structural analysis proved that 5d crystallizes in the space group \documentclass{article}\pagestyle{empty}\begin{document}$ P\bar 1 $\end{document} with Z = 2. Under CO pressure 5d was degraded to the selenophene 6.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290811
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