Stannoles bearing dialkylboryl groups in 3-position react with 1-phospha-1-alkynes P≡C-tBu (1) and P≡C-CH2tBu (2) by [4 + 2] cycloaddition and elimination of stannylene to give phosphabenzenes in high yield. The stannylenes oligomerise to give [R12Sn]nwith n ≥ 7 (R = Me, Et, -(CH2)5-or, in the case of R1=tBu, react with the stannole itself. All phosphabenzenes are characterised by their consistent sets of NMR data. The absolute signs of the coupling constantsnJ(31P,1H),nJ(31P,13C),2J(31P,29Si) and2J(119Sn,31P) were determined by appropriate 1D and 2D NMR experiments.
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