In our laboratory, we have recently made significant strides in leveraging the power of flow chemistry to directly harness and manage various gaseous reagents. Within this research framework, we have unveiled a modular flow platform capable of producing SO2F2 from readily available, bench-stable chemicals such as KF and SO2Cl2 (Scheme 1A) through a Cl-F exchange process. The intrinsic containment properties of this flow system ensure the safe and controlled generation of the gaseous reagent, while also facilitating precise dosing of the reactive gas. , This breakthrough has enabled the execution of a diverse range of SuFEx (Sulfur(VI) Fluoride Exchange) ligations on a wide spectrum of compounds, including small molecules, biorelevant compounds, peptides, and proteins. Recently, we wondered whether we could extend the range of gases generated through this microfluidic device to thionyl fluoride, SOF2. This gas has long been overlooked as a deoxyfluorinating reagent due to safety concerns associated with its handling and toxicity. Only recently, work by Sammis and co-workers demonstrated how stock solutions of this gas could be produced through an ex situ approach. However, this strategy requires multiple manipulations due to the batch setup, and forms the undesired F/Cl mixed species SOFCl and stoichiometric amounts of HCl, limiting its practicality and potential applications. Our interest in generating SOF2 stemmed from its ability to swiftly convert abundant carboxylic acids into acyl fluorides. This stands in stark contrast to the limitations of low atom economy, limited functional group tolerability, and high costs associated with the use of engineered reagents like DAST, cyanuric fluoride, Deoxo-Fluor, or Fluolead, among others (Scheme 1B). Acyl fluorides are in fact an enticing class of carboxylic acid derivatives known for their synthetic utility as well as their enhanced stability and peculiar reactivity compared to their chloride analogs. Acyl fluorides are isolable and exhibit increased stability with respect to other acyl halides, and yet require mild reaction conditions to engage in diverse synthetic transformations. Thus, when reacted with nucleophiles, they offer a straightforward route to a wide range of valuable products such as esters, amides, or thioesters, almost regardless of the steric and electronic properties. Herein, we report the development of a strategy that harnesses the power of a microfluidic device to form thionyl fluoride and swiftly use it to convert carboxylic acids into acyl fluorides (Scheme 1C). Furthermore, we demonstrate the feasibility of a multistep flow approach where the carboxylic acids are directly converted into amides, esters, thioesters, and ketones.