Fluorination of Alkyl‐Substituted Ylides With HBF ₄ •Et ₂ O

The development of a rapid and efficient fluorination reaction of difluoroalkyl‐ and alkyl‐substituted ylides employing HBF ₄ •Et ₂ O as the fluorinating agent is reported. This operationally simple protocol typically proceeds to full conversion within 5–30 min at room temperature or slightly above, affording a diverse array of monofluoroalkanes and trifluoromethylated alkanes in good to excellent yields. The exceptionally short reaction time, mild conditions, and use of a readily available fluorinating source render this method particularly attractive for applications that require rapid fluorine incorporation, such as the preparation of PET‐CT tracers.