Study On Green Synthesis Of Diethyl Malonate And Ethyl Acetoacetate

Diethyl malonate(DEM) and ethyl acetoacetate(ACE) are important fine chemical feedstocks, which are widely used in pharmaceutical, polyester, dyestuff and perfume industries. The synthetic methods of DEM are mainly included the method of sodium cyanid, hydroxylation, transesterification, esterification et al. Nowadays in our country, most of it is produced by sodium cyanide traditionally. This method has a long technological process and a low yield, especially cyanides which is highly toxic used in the process can lead to environmental pollutions. The synthetic methods of ethyl acetoacetate are mainly included diethenone process and ester condensation. In this paper, by the study on Claisen ester condensation, DEM and ethyl acetoacetate have been successfully synthesized. Effects of many factors such as activation time, solvent type, feed ratio, pressure on the conversion rate, selectivity and yield of DEM and ethyl acetoacetate were investigated.Based on experiments, a proper process has been found. It follows that 8 distillation trays, HSCM used as catalyst, DL-2 used as solvent, the reaction time 5 hours, the material ratio of n(DEC)/n(EA) was 1:5, the reflux ratio was 10:5, at atmospheric pressure. Under this process conditions, the yield of DEM can reach 39.72%, the yield of ethyl acetoacetate can reach 22.48%. The separation of overhead product was simulated by ASPEN PLUS. The yield of EA can reach 98.95%.