Milligram-scale, temperature-controlled ball milling to provide an informed basis for scale-up to reactive extrusion
Milligram-scale, temperature-controlled ball milling to provide an informed basis for scale-up to reactive extrusion
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DOI：
10.1039/d1gc02174e
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发表时间：
2021-09-30
期刊：
影响因子：
9.8
通讯作者：
Mack, James
中科院分区：
文献类型：
--
作者：
Andersen, Joel;Starbuck, Hunter;Mack, James
在过去的几年里，化学家和工程师已经确定了使用双螺杆挤出机进行大规模有机化学机械化学的效用。该设备非常方便，因为它是几个相关行业熟悉的配方，它也配备了良好的温度控制和材料的强烈研磨。然而，机械化学的研发规模与常规合成一样：毫克。这些毫克级的反应在间歇式反应器中进行，通常是球磨机。可商购的球磨机米尔斯不具有严格的温度控制，限制了可以获得的信息以可靠地通知放大过程。这项工作使用内部修改，温度控制，球磨机，以弥补知识差距，关于可预测的，消息灵通的，经济的，可靠的机械化学放大。包括在这项工作是亲核芳香取代的第一个挤出的例子。
Over the last several years, chemists and engineers have identified the utility of using twin-screw extruders for performing large-scale organic chemistry mechanochemically. This equipment is convenient as it is familiar to several relevant industries for its use in formulation, and it is also well-equipped for temperature control and intense grinding of materials. However, the research and development scale of mechanochemistry is just like that of conventional synthesis: milligrams. These milligram-scale reactions are performed in batch-type reactors, often a ball mill. Commercially available ball mills do not have strict temperature control, limiting the information that can be obtained to inform the scale-up process reliably. This work uses an in-house modified, temperature-controlled, ball mill to bridge the knowledge gap regarding predictable, well-informed, economical, and reliable mechanochemical scale-ups. Included in this work is the first extrusion example of a nucleophilic aromatic substitution.