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Bis‐TMS protected C,C‐diacetylenic phosphaalkene (A2PA) 1 (Mes*PC(C≡CTMS)2; Mes*=2,4,6‐tBu3Ph) has been used as a building block for the construction of butadiyne‐expanded dendralene fragments in which phosphaalkenes feature as exotopic double bonds. Treatment of 1 with CuCl gives rise to a CuI acetylide that is selectively formed at the acetylene trans to the Mes* group. The cis‐TMS‐acetylene engages...
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