The highest homologue of the [n]phenylenes thus far isolated, the title compound 1, is a deep‐red, extremely air‐sensitive crystalline compound. A newly developed strategy for the synthesis of such hydrocarbons has proven to be extremely efficient: cocyclization of tetraethynylbenzene with the hexa‐triyne iPr3SiCCCCCCSiiPr3 leads to a [3]phenylene, which, in turn, is likewise a tetraethynyl compound and can thus be employed in renewed cocyclizations.
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