João A. F. Silva, Mônica F. Z. J. Toledo, Flávia Manarin, João H. de Araujo‐Neto, Milene M. Hornink, Hélio A. Stefani
We developed an efficient methodology for synthesizing C ‐acyl‐glycosyl sulfonamides via a carbonylative coupling reaction, using 1‐iodo‐glycals as substrates. A wide range of aromatic, heteroaromatic, and aliphatic sulfonamides was explored, employing Mo(CO) 6 as a safe, solid source of carbon monoxide gas. This approach enabled the preparation of novel glycosyl sulfonamides featuring a C ‐acyl‐linked framework under mild reaction conditions, achieving good to excellent yields.