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Herein, a more practical and efficient synthesis protocol for the preparation of uniform rod‐like oligo(1,4‐phenylene ethynylene)s (OPE)s is presented. Applying an iterative reaction cycle consisting of a decarboxylative coupling reaction and a saponification of an alkynyl carboxylic ester, a uniform pentamer is obtained in ten steps with 14% overall yield. The copper‐free conditions prevent homocoupling...
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