Rhodium‐Catalyzed [3+2]‐Cycloaddition of in‐situ Generated Nitrile Ylides with Nitrosoarenes

Herein we report the rhodium‐catalyzed one‐pot three‐component reaction of diazo compounds, nitriles, and nitrosoarenes to construct 2,5‐dihydro‐1,2,4‐oxadiazole derivatives. Mechanistic studies indicate that the transformation may proceed through the formation of nitrile ylides intermediates, which then undergo [3+2]‐cycloaddition with nitrosoarenes. The strategy exhibits several synthetic advantages, including operational simplicity, good functional group tolerance, and scalability.