Abstract Ethers are of central importance in the fields of biomass, energy, and organic chemistry. Herein, a novel cobalt‐catalyzed carbonylative coupling of ethers with amines to construct α‐carbonylated ethers has been achieved. Remarkably, Alfuzosin, a medicine for treatment of benign prostatic hyperplasia (BPH), can be synthesized by this process straightforwardly. Notably, this protocol presents the first example on the direct carbonylative reaction of ethers.
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