Scale-Up of Microwave-Assisted Reactions in a Multimode Bench-Top Reactor

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• 作者：Doris Dallinger ; Hansjo虉rg Lehmann ; Jonathan D. Moseley ; Alexander Stadler ; C. Oliver Kappe
• 刊名：Organic Process Research & Development
• 出版年：2011
• 出版时间：July 15, 2011
• 年：2011
• 卷：15
• 期：4
• 页码：841-854
• 全文大小：1191K
• 年卷期：v.15,no.4(July 15, 2011)
• ISSN：1520-586X

文摘

An evaluation of a new bench-top microwave batch reactor that uses a single 1 L reaction vessel is presented. Several microwave-assisted organic reactions have been scaled-up, including Newman Kwart and Diels鈥揂lder reactions, Pd-catalyzed cross-couplings, heterocycle synthesis, aromatic substitution, and a Knoevenagel condensation. A range of different solvents (high and low microwave absorbing), varying reaction times (4 s up to 2 h), and temperatures (120鈥?50 掳C) have been explored in these investigations. For all studied transformations, it was possible to perform a direct scale-up (up to 720 mL reaction volume) without changing the previously optimized reaction conditions achieved in a laboratory-scale single-mode microwave instrument (2鈥?0 mL processing volume), obtaining similar isolated product yields. A scalability up to 360-fold, when moving from 3 mmol up to 1.08 mol, was demonstrated, and isolated product yields up to 300 g (2.5 mol scale) in a single run could be accomplished, providing the potential for a kilogram output per day for specific transformations by performing multiple sequential runs.