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Research of technique for synthesizing carbonyl diethyl malonate
Authors:Houying Gui  Liuyu Dong  Qiuming Zhou  Xinming Hu
Institution:GUI Houying,DONG Liuyu,ZHOU Qiuming,HU Xinming School of Sciences,Wuhan University of Technology,Wuhan 430070,Hubei,China
Abstract:Diethyl malonate being an initial raw material, processed with chlorination-replacement-desalination-vacuum rectification, is used to produce carbonyl diethyl malonate. An experiment for optimization determines that the best reaction condition was: ① reaction for 7 h at 10 °C with mole-ratio being 2.4:1 between chloride and raw material (diethyl malonate); ② reaction for 4.5 h at 118 °C with mole-ratio being 1.2:1 between the anhydrous sodium acetate and intermediate I. The final product carbonyl diethyl malonate recovery ratio reaches up to as high as 79.12% with a purity of 96.4%, which meets the market requirement. This synthesis technique has the advantages of simple process, moderate reaction conditions, high yield and low cost, being suitable for industrial scale production.
Keywords:diethyl malonate  chlorination  replacement  desalination  rectification  carbonyl diethyl malonate  
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