High‐Energy Ball Milling Enables an Ultra‐Fast Wittig Olefination Under Ambient and Solvent‐free Conditions

30 Seconds to success!—The Wittig reaction, a fundamental and extensively utilized reaction in organic chemistry, enables the efficient conversion of carbonyl compounds to olefins using phosphonium salts. Traditionally, meticulous reaction setup, including the pre‐formation of a reactive ylide species via deprotonation of a phosphonium salt, is crucial for achieving high‐yielding reactions under classical solution‐based conditions. In this report, we present an unprecedented protocol for an ultra‐fast mechanically induced Wittig reaction under solvent‐free and ambient conditions, often eliminating the need for tedious ylide pre‐formation under strict air and moisture exclusion. A range of aldehydes and ketones were reacted with diverse phosphonium salts under high‐energy ball milling conditions, frequently giving access to the respective olefins in only 30 seconds. We present a protocol for a solvent‐free mechanically induced Wittig olefination under ambient conditions often without the need of ylide pre‐formation with a 30 seconds reaction time under high‐energy ball milling conditions.