Mechanochemical Electrophilic Fluorination of Liquid Beta-Ketoesters

Analysis of an improved substrate scope for the mechanochemical electrophilic fluorination of dicarbonyls is reported. The applicable substrates have now been broadened to include liquid b-ketoesters. Key to this capability is the inclusion of a grinding auxiliary (NaCl) to improve mass transfer and prevent pasting or gumming of the reaction mixture. Notably, the use of a small amount of acetonitrile is ciritical to increasing the rate of reaction, ensuring complete consumption of starting materials during the short reaction times as well as improving the selectivity for the monofluorinated product in the mill. The data here contains a selection of 1H, 13C, 19F NMR data, as well as IR, MS and any relevant chromatography information. Some files may be processed in advance and deposited and some may require access to typical processing tools for data of this type.本研究报道了二羰基化合物机械化学亲电氟化反应底物范围的优化拓展工作。当前该反应的适用底物已拓展至液态β-酮酯。实现该底物适配范围拓展的关键在于引入研磨助剂（氯化钠，NaCl），以改善传质效果并防止反应混合物结块或黏结。值得注意的是，添加少量乙腈对于提升反应速率、确保短反应时间内原料完全转化，以及提升机械化学反应体系中单氟化产物的选择性均至关重要。本数据集包含精选的1H、13C、19F核磁共振波谱（NMR）数据，同时涵盖红外光谱（IR）、质谱（MS）及相关色谱分析数据。部分文件已提前完成处理并归档，其余文件则需借助针对此类数据的常规处理工具方可完成解析。