A highly efficient protocol for the β‐arylation of carboxylic amides by aryl iodides under PdCl2(CH3CN)2/CsOAc catalysis was developed. This method was found to tolerate a broad scope of substrates and was successfully employed in the preparation of a variety of β‐aryl α‐amino and γ‐amino acid derivatives. The utility of this method was further illustrated in the synthesis of the psychotropic drug (±)‐phenibut and β‐aryl bile acid analogues.
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