The continuous synthesis of Grignard reagents has been investigated under continuous processing conditions using Mg turnings at variable liquid throughputs and concentrations. A novel process window easily accessible through continuous processing was employed, namely, using a large molar access of Mg turnings within the reactor and achieving Mg activation by mechanical means. A laboratory and a 10-fold-increased pilot-scale reactor setup were built and evaluated, including integrated inline analytics via ATR-IR measurements. The main goal of this work was to explore the full potential of classic Grignard reagent formation through the use of scalable flow chemistry and to allow for fast and safe process optimization. It was found that on both the laboratory and pilot scales, full conversion of the employed halides could be achieved with a single passage through the reactor. Furthermore, Grignard reagent yields of 89–100% were reached on the laboratory scale.

中文翻译：

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从原位活化镁金属可扩展连续合成格氏试剂

已经在连续工艺条件下使用可变液体通过量和浓度的Mg车削在连续加工条件下研究了格氏试剂的连续合成。采用了一种易于通过连续加工获得的新颖的工艺窗口，即在反应器内使用大量摩尔的Mg车削进入，并通过机械手段实现Mg的活化。建立并评估了实验室和中试规模的反应堆，其规模增加了10倍，包括通过ATR-IR测量进行的集成在线分析。这项工作的主要目的是通过使用可扩展的流动化学来探索经典格利雅试剂形成的全部潜力，并实现快速安全的工艺优化。结果发现，无论是实验室规模还是中试规模，只需通过反应器一次，就可以实现所用卤化物的完全转化。此外，在实验室规模上，格氏试剂的产率达到89-100％。