Nie Honggang, Wei Zhenwei, Qiu Lingqi, Chen Xingshuo, Holden Dylan T, Cooks R Graham
Aston Labs, Department of Chemistry, Purdue University 560 Oval Drive West Lafayette IN 47906-1393 USA
Beijing National Laboratory for Molecular Sciences, College of Chemistry and Molecular Engineering, Peking University Beijing 100871 P. R. China.
Chem Sci. 2020 Jan 29;11(9):2356-2361. doi: 10.1039/c9sc06265c.
A closed system has been designed to perform microdroplet/thin film reactions with solvent recycling capabilities for gram-scale chemical synthesis. Claisen-Schmidt, Schiff base, Katritzky and Suzuki coupling reactions show acceleration factors relative to bulk of 15 to 7700 times in this droplet spray system. These values are much larger than those reported previously for the same reactions in microdroplet/thin film reaction systems. The solvent recycling mode of the new system significantly improves the reaction yield, especially for reactions with smaller reaction acceleration factors. The microdroplet/thin film reaction yield improved on recycling from 33% to 86% and from 32% to 72% for the Katritzky and Suzuki coupling reactions, respectively. The Claisen-Schmidt reaction was chosen to test the capability of this system in gram scale syntheses and rates of 3.18 g per h and an isolated yield of 87% were achieved.
已设计出一种封闭系统，用于进行微滴/薄膜反应，并具备溶剂循环能力，可用于克级化学合成。在该液滴喷雾系统中，克莱森-施密特反应、席夫碱反应、卡特里茨基反应和铃木偶联反应相对于本体反应的加速因子为15至7700倍。这些值远大于先前在微滴/薄膜反应系统中报道的相同反应的值。新系统的溶剂循环模式显著提高了反应产率，特别是对于反应加速因子较小的反应。对于卡特里茨基反应和铃木偶联反应，微滴/薄膜反应产率在循环后分别从33%提高到86%和从32%提高到72%。选择克莱森-施密特反应来测试该系统在克级合成中的能力，实现了每小时3.18克的速率和87%的分离产率。
