Understanding of two-stage continuous microreaction technology for in-situ generation and consecutive conversion of diazomethane

Abstract

Abstract Microreaction technology (MRT) offers a safe way to deliver useful, highly active but hazardous diazomethane on demand within a closed system and then realize in-situ conversion to the desired product. In this work, the two-stage MRT is employed for the integrated synthesis of diazomethane and its consecutive conversion with benzoic acid, and the key factors resulting in the low product yield are investigated in depth. Extensive optimization of reaction conditions (e.g., the total flow rate, residence time, temperature and reactants ratio), solvent selection as well as heat management are performed. Special attention has to be devoted to the significantly detrimental effect of water solvent on the product yield. These results provide some fundamental understanding of the interlinked reaction chemistry and engineering, which could guide the MRT development for continuous operation when using hazardous compounds.