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Cyanohydroxycarbonylation of α-keto alkynes in the presence of potassium ferrocyanide, carbon monoxide, and potassium cyanide in water, under moderate reaction conditions of pressure and temperature, affords unsaturated carboxylactams. The complex [FeII(CO)2(CN)4]2-, formed “in situ” from K4Fe(CN)6, appears to be an active species in the reaction, and a plausible mechanism was proposed for the formation of carboxylactams.