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 t...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 ℃ with mole-ratio being 2.4 ＂ 1 between chloride and raw material （diethyl malonate）; （2 reaction for 4.5 h at 118 ℃ with mole-ratio being 1.2 ： 1 between the anhydrous sodium acetate and intermediate I. The final product carbonyl diethyl rnalonate 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.展开更多
基金Supported by the Innovation Fund for Technology Based Firms(10C26224212340)
文摘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 ℃ with mole-ratio being 2.4 ＂ 1 between chloride and raw material （diethyl malonate）; （2 reaction for 4.5 h at 118 ℃ with mole-ratio being 1.2 ： 1 between the anhydrous sodium acetate and intermediate I. The final product carbonyl diethyl rnalonate 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.
