Synthesis and structure of an acyclic dialkylstannylene
Autor: | Izod Keith, Wills Corinne, Probert Michael R., Harrington Ross W. |
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Jazyk: | angličtina |
Rok vydání: | 2014 |
Předmět: | |
Zdroj: | Main Group Metal Chemistry, Vol 37, Iss 5-6, Pp 113-117 (2014) |
Druh dokumentu: | article |
ISSN: | 0792-1241 2191-0219 |
DOI: | 10.1515/mgmc-2014-0028 |
Popis: | The reaction between iPr2 PCl and one equivalent of MeMgBr, followed by one equivalent of BH3·SMe2, gives the phosphine-borane iPr2 P(BH3)Me (4). Treatment of 4 with nBuLi, followed by Me3 SiCl, gives the sterically demanding phosphine-borane {iPr2 P(BH3)}(Me3 Si)CH2 (5) in good yield. Metalation of 5 with nBuLi yields {iPr2 P(BH3)}(Me3 Si)CHLi (6), which was crystallised as the TMEDA adduct [{iPr2 P(BH3)}(Me3 Si)CH]Li(TMEDA) (6a) and characterised by X-ray crystallography [TMEDA = N,N,N′,N′-tetramethylethylenediamine]. The reaction between two equivalents of in situ-generated 6 and Cp2 Sn in toluene gives the dialkylstannylene [{iPr2 P(BH3)}(Me3 Si)CH]2 Sn (7), which was crystallised from methylcyclohexane/THF as the rac diastereomer. X-ray crystallography reveals that stabilisation of the Sn centre in 7 is afforded by two agostic-type B-H…Sn interactions, one from each BH3 group. |
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