FeCl3/K2S2O8/Et3SiH System‐Mediated α‐Methylation of β‐Ketosulfones with DMF

Abstract FeCl 3 /K 2 S 2 O 8 /Et 3 SiH system‐mediated α‐methylation of β‐ketosulfones with N , N ‐dimethylformamide (DMF) was developed. In the overall process, DMF takes up the role of one methyl group in the generation of α‐methyl β‐ketosulfones via single carbon−carbon (C−C) bond formation under reflux conditions. Herein, a plausible reaction mechanism is proposed.