二乙二醇丙酸甲酯的合成与结构表征

采用二乙二醇和丙酸甲酯为主要原料,以钾为催化剂,在通N_2气保护的条件下合成二乙二醇丙酸甲酯,用离子排阻高效液相色谱法对合成的二乙二醇丙酸甲酯进行定量分析。最佳合成条件:二乙二醇与丙酸甲酯的物质的量比为1∶2,催化剂的质量为反应物二乙二醇质量的1.5%,于25℃条件下反应24 h,产物经硅胶柱分离、乙酸乙酯梯度洗脱,然后干燥,制得二乙二醇丙酸甲酯成品,收率为61.5%,纯度达99.5%。用FT-IR,~1H–NMR,GC–MS法对二乙二醇丙酸甲酯的分子结构进行了确证。

Synthesis and Structure Characterization of Methyl 3-[2-(2-Hydroxyethoxy)Ethoxy] Propanoate

Diethylene glycol(PEG2) and methyl propionate as main raw materials, potassium as the catalyst and under the conditions of N2 gas protection, synthesis of diethylene glycol methyl propionate was developed. Quantitative analysis of PEG3–CO2Me was carried out by using ion exclusion chromatography with high performance liquid chromatography. The optimal synthesis conditions were found that molar ratio of diethylene glycol and methyl propionate was 1∶2, catalyst mass was 1.5% of PEG2 mass, reaction time was 24 h at 25℃, separated by silica gel column, eluted with ethyl acetate, the target product of PEG3–CO2Me was obtained. The yield rate was 61.5% with the purity of 99.5%. The molecular structure of diethylene glycol methyl propionate was syndrome by FT-IR,1H NMR, GC–MS.