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  • Chemistry  (2)
  • Inorganic Chemistry  (2)
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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 118 (1985), S. 3227-3240 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: λ5-Di- and -Triazaphospholines - Synthesis, Isomerization, and DecompositionThe reaction of amino[(trimethylsilyl)methylene]thioxophosphorane 1 with diazoalkanes leads to Δ1-diazaphospholines 3, 7, 11, and 12. These sensitive compounds are stabilized by 1,3-migration of a trimethylsilyl group, where 3 and 7 end in the Δ2-diazaphospholines 4 and 8 and 11 and 12 decompose by [1 + 4]cycloreversion to give the azines 14 and 15 as well as aminothioxophosphane intermediate 13. 13 could be trapped by reaction with diazoalkanes as aminomethylenethioxophosphoranes (18 and 19). The corresponding phosphane system 20 and 21 is available by reduction of 18 and 19, respectively, with triphenylphosphane. tert-Butyl azide (22) and 1 form triazaphospholine 23, which isomerizes thermally by silyl migration to give 24. Photochemically induced elimination of N2 leads to the λ5-azaphosphiridine 25; this system is also accessible by reaction of aminoiminothioxophosphorane 26 with diazomethane. In contrast, thermal reaction of trimethylsilyl azide (30) and 1 results in a λ5-thiaphosphirane 31. Compounds of this type (31, 32) can also be synthesized by [1 + 2]cycloaddition of sulfur and the corresponding iminomethylenephosphorane. - The X-ray structure analysis of the Δ2-diazaphospholine 5 is described, NMR data and decomposition of di- and triazaphospholines are discussed.
    Notes: Amino[(trimethylsilyl)methylen]thioxophosphoran 1 reagiert mit Diazoalkanen zu den Δ1-Diazaphospholenen 3, 7, 11 und 12. Diese stabilisieren sich unter 1,3-Trimethylsilyl-Verschiebung zu den Δ2-Diazaphospholenen 4 und 8 bzw. zerfallen unter [1 + 4]-Cycloreversion zu Azin (14 und 15) und dem Aminothioxophosphan 13. 13 konnte durch Reaktion mit Diazoalkan als Aminomethylenthioxophosphoran (18 und 19) abgefangen werden. Durch Entschwefelung von 18 bzw. 19 mittels Triphenylphosphan ist das entsprechende Phosphan-System 20 bzw. 21 zugänglich. tert-Butylazid (22) reagiert mit 1 zum Triazaphospholen 23, das thermisch unter Trimethylsilyl-Wanderung zu 24 isomerisiert und photochemisch unter N2-Eliminierung das λ5-Phosphiridin 25 liefert, ein Verbindungssystem, das ebenfalls durch Umsetzung eines Aminoiminothioxophosphorans (26) mit Diazomethan zugänglich ist. Bei der thermischen Reaktion von 1 und Trimethylsilylazid (30) wird hingegen das λ5-Thiaphosphiran 31 erhalten. Verbindungen dieses Typs (31, 32) sind auch durch Schwefelung der entsprechenden Iminomethylenphosphorane zugänglich. - Die Röntgenstrukturanalyse des durch partielle Hydrolyse von 4 erhaltenen Δ2-Diazaphospholens 5 wird angegeben, und die NMR-Daten sowie der Zerfall der Di- und Triazaphospholene werden diskutiert.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0009-2940
    Keywords: 1,2-Dihydro-1,3,2λ5,4λ5-diazadiphosphete ; Isomerization ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,2-Dihydro-1,3,2λ5,4λ5-diazadiphosphete - Synthesis, Structure and Isomerization to the „Inner Salt“ of 1,3,2,4λ5-Diazadiphosphetan-2-ium HydroxideThe photochemical reaction of the azidophosphane (iPr2N)2PN3 (1) with the tetraazaphospholene (3) and the bis(imino)phosphorane (Me3Si)2NP(=NSiMe3)2 (6) proceeds by elimination of N2 to yield (5) and by 1,3-silyl group shift to furnish (8) the structures of which were determined by means of NMR data and, in the case of 5, additionally by X-ray structure analysis.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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