On Demand Flow Platform for the Generation of Anhydrous Dinitrogen Trioxide and Its Further Use in <i>N</i> ‐Nitrosative Reactions

Dinitrogen trioxide (N2O3) is a powerful and efficient nitrosating agent that comes with an unprecedented atom economy. However, the synthetic application of N2O3 still underdeveloped mostly due to its inherent instability lack reliable protocols for preparation. This paper presents open-source setup procedure on-demand generation anhydrous solution (up 1 M), which can be further used reactions under batch flow conditions. The accuracy stability concentration are guaranteed absence head-space in synchronization gas flows. reliability this protocol demonstrated by >30 worked examples nitrosative synthesis heterocycles—a library structurally diverse benzotriazoles sydnones. Kinetic mechanistic aspects N-nitrosative steps also explored.