Ethyl diazoacetate (EDA) synthesis using ethyl glycinate hydrochloride (EGH) and sodium nitrite (SN) as starting materials involves the diazo reaction (main reaction) and EDA decomposition reaction (side reaction). In this work, the main reaction is assumed to be faster than the side reaction; therefore, we determine the side reaction kinetics and the reaction heat of the side reaction and main reaction by processing the calorimetric data in segmentation. We then establish an adiabatic microchemical system with in-situ infrared temperature measuring accessories. We determined the time profile of the adiabatic temperature rise and derived the kinetic equation of the main reaction by a multi-parameter numerical computational regressive analysis using a Monte Carlo method. Combining the kinetic equations of the main reaction and side reaction, the continuous EDA synthesis process in an adiabatic microchemical system was modelled and well predicted. Compared with a semi-batched industrial process, the newly developed and designable EDA synthesis strategy increased the EDA yield from 85% to 95% and decreased the residence time from several hours to tens of seconds. (C) 2015 Elsevier B.V. All rights reserved.