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Polyarylacetylene resins have received great attention due to their outstanding heat resistance, while the absence of an efficient method to produce their monomer, p‐diethynylbenzene (p‐DEB), has discouraged their commercial development. Industrial production of p‐DEB consists of bromination and dehydrobromination in a semi‐batch reactor, state of the art yield from which is only 70%–75%. Herein,...