Résumé
In its ongoing development, mechanochemistry is becoming equipped with additional energy inputs such as light. In this work we demonstrate a proof‐of‐principle setup for real‐time in situ Raman monitoring of photomechanochemical reactions. Using photoisomerization of azobenzenes, and photolysis of adamantane diazirine as model reactions, we show that multiple photoisomerization cycles can be performed and monitored in a ball mill, and highlight reaction selectivity that can be achieved by photomechanochemistry.