臭氧氧化法合成乙醛酸乙酯

以马来酸二乙酯为原料,乙酸乙酯作溶剂,采用臭氧氧化和加氢还原工艺合成了乙醛酸乙酯,获得的较佳工艺条件为:n(乙酸乙酯)∶n(马来酸二乙酯)=15∶1,臭氧化温度20℃,反应时间80 min;以Pd/C作催化剂,m(Pd/C)∶m(马来酸二乙酯)=0.09∶1,氢气压力4 MPa,还原温度25℃,还原时间5 h。在该条件下,马来酸二乙酯的转化率达100%,产物收率≥89.0%,产物色谱纯度≥96.6%。采用IR和1HNMR技术对产物结构进行了表征。

Synthesis of Ethyl Glyoxylate by Ozonization

Ethyl glyoxylate was synthesized by ozonization and hydro-reduction using diethyl maleate as raw material and ethyl acetate as solvent.The ascertained optimum conditions were n(ethyl acetate):n(diethyl maleate)=15:1,ozonization temperature 20 ℃,ozonization time 80 min;using Pd/C as hydrogenation catalyst,m(Pd/C):m(diethyl maleate)=0.09:1,hydrogen pressure 4 MPa,reduction time 5 h,reduction temperature 25 ℃.Under the above conditions,the conversion of diethyl maleate was almost 100%,and the yield of ethyl glyoxylate was ≥89.0% with a purity of more than 96.6%.The structure of the obtained product was characterized by means of IR and 1HNMR.