Copper‐Free One‐Pot Sonogashira‐Type Coupling for the Efficient Preparation of Symmetric Diarylalkyne Ligands for Metal‐Organic Cages**

The often time-consuming and challenging multi-step synthesis of ligands for metal-organic cages is a limiting factor the discovery application new cages. We report highly efficient copper-free one-pot Sonogashira-type coupling preparation symmetric diarylalkyne on both small large scale; bipyridine- benzimidazole-based self-assembly Co4L6 were synthesized in short reaction times high isolated yields directly from aryl halide precursors. This method reduces synthetic burden ligand will facilitate with additional functionality applications their corresponding