In the context of the growing interest of the scientific community for the development of sustainable synthetic strategies to access aromatic structures, we present a practical and metal-free approach to (hetero)biaryls which exploits the advantages of multicomponent reactions in sustainable solvents. In situ acid-catalysed generation of (hetero)aryl acetoxy dienes from the corresponding (hetero)arylidene acetones in a metal vessel, followed by Diels-Alder reaction using an electronpoor alkyne as dienophile, delivers the expected aromatic prod- [a] 7711 Scheme 1. Thermal activation of alkynes in multicomponent metal-free synthesis of (hetero)aryl-substituted phenyls in metal vessel. 7712 field of research under hyperbaric, thermal and microwave activation, [48][49][50] due to the scarce reactivity of this compound with consequently unsatisfying yields. [51] Eur.
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