Stannoles bearing dialkylboryl groups in 3-position react with 1-phospha-1-alkynes P≡CtBu (1) and P≡CCH2tBu (2) by [4 + 2] cycloaddition and elimination of stannylene to give phosphabenzenes in high yield. The stannylenes oligomerise to give [R12Sn]n with n ≥ 7 (R Me, Et, -(CH2)5− or, in the case of R1 = tBu, react with the stannole itself. All phosphabenzenes are characterized by their consistent sets of NMR data. The absolute signs of the coupling constants nJ(31P, 1H), nJ(31P, 13C), 2J(31P, 29Si) and 2J(119Sn, 31P) were determined by appropriate ID and 2D NMR experiments.
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