A synthesis process of 5-fluoro-2-nitrobenzotrifluoride was achieved in a continuous-flow millireactor system through the nitration of 3-fluorobenzotrifluoride using the mixed acid as a nitrating agent. The process safety was evaluated based on the temperature rise with the use of Reaction Calorimeter and Differential Scanning Calorimetry. The mass transfer limitation for this nitration process in the millireactor was evaluated. Effects of the composition of the mixed acid, the molar ratio of nitric acid to the substrate, the residence time, and the temperature on the reaction performance in the millireactor were studied in order to obtain optimal operational conditions. A heat transfer assessment was made to discuss the effects of the residence time and the inner diameter on the temperature distribution and the substrate conversion. Compared with the traditional batch reactor, the flow reactor could achieve better control over impurity and higher process efficiency because of its enhanced mass and heat transfer rates under the optimized conditions. This continuous-flow synthesis strategy would be beneficial for the commercial manufacturing of fine chemicals and pharmaceutical intermediates with the involvement of nitration.

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通过使用混合酸作为硝化剂硝化3-氟代苯并三氟乙烷，在连续流动毫反应器系统中实现了5-氟代-2-硝基苯并三氟乙烷的合成过程。使用反应量热仪和差示扫描量热法，基于温度升高来评估过程安全性。评估了毫反应器中该硝化过程的传质极限。研究了混合酸的组成，硝酸与底物的摩尔比，停留时间和温度对毫反应器中反应性能的影响，以获得最佳操作条件。进行传热评估以讨论停留时间和内径对温度分布和基材转化率的影响。与传统的间歇式反应器相比，由于在优化条件下提高了质量和传热率，因此流动反应器可以更好地控制杂质并提高处理效率。这种连续流合成策略对于硝化作用下的精细化学品和医药中间体的商业化生产将是有益的。

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