Continuous synthetic process for ethyl diazoacetate
YUE Jia-wei1,2, GU Shun-lin1,2, LIU Jian-wu1,2, ZHU Jia-hui1,2, LI Meng-jin1,2, ZHANG Yue2, YAN Sheng-hu1,2
1. School of Pharmacy & School of Medicine, Changzhou University, Changzhou 213164, China; 2. Continuous Flow Engineering Laboratory of National Petroleum and Chemical Industry, Changzhou 213164, China
Abstract: A continuous flow synthetic process for ethyl diazoacetate is studied in a microchannel reactor by using glycine ethyl ester hydrochloride and sodium nitrite as raw materials.The effects of the dosage of sodium nitrite,reaction temperature,acid dosage and residence time on the reaction yield are investigated.Since this reaction is highly exothermic and the product is unstable under higher temperature,traditional kettle batch operation is very easy to cause locally overheated,leaving major hidden danger and leading to product decomposition.Ordinary pipeline reactors are hard to overcome mass transfer obstacle due to heterogeneity,resulting in lower yield.Microchannel reactors maintain good heat transfer efficiency while fully break through the phase interface obstacle to ensure the sufficient mixing of heterogeneous reaction liquids.So microchannel reactors are very suitable for the development of this synthetic process.By means of the advantages of the microchannel reactor,novel process for ethyl diazoacetate is developed and the process conditions are optimized in order to improve the reaction efficiency and yields.