AbstractSymmetric and unsymmetric diaroyl‐S,N‐ketene acetals can be readily accessed in consecutive syntheses in good to excellent yields by exploiting the inherent nucleophilic character of the methine position. Different aroyl‐S,N‐ketene acetals as well as acid chlorides yield a library of 19 diaroyl compounds with substitution and linker pattern‐tunable emission properties, leading to a significant red‐shift of emission in the solid and aggregated state, which was thoroughly investigated. Additionally, the stability of the luminescent aggregates is highly increased. In a follow‐up one‐pot procedure, pyrazolo‐S,N‐ketene acetals can easily be accessed employing a nucleophilic cyclocondensation.

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