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An efficient transition metal‐free approach to achieve the selective cleavage of the α‐carbonyl C(sp3)−H bond in alkyl esters by using inexpensive, low‐toxic, and insensitive perfluoroalkyl iodide as the radical initiator has been developed. A variety of enamides, N‐heterocycles, amides, thiophenols, and phenols could be successfully incorporated into functionalized alkyl groups by intermolecular...
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