β-衣康酸单甲酯的合成工艺研究

以衣康酸和甲醇为主要原料,乙酰氯为催化剂,研究了β衣康酸单甲酯的合成工艺。通过正交试验考察了反应物摩尔配比、反应时间、反应温度、溶剂量以及催化剂等因素对反应结果的影响,得到了最佳合成工艺条件,即n(衣康酸):n(甲醇)∶n(乙酰氯)=1∶3.5∶0.042,反应温度65℃,反应时间0.5h,产品收率和质量分数分别达到86%和97%。采用GCMS确定了产品β衣康酸单甲酯及主要杂质的结构。

Studies on Synthesis of Beta-monomethyl Itaconate

Beta-monomethyl itaconate was synthesized by using itaconic acid and methyl alcohol as raw materials and using acetyl chloride as catalyst. The effects of molar ratio of reactants, reaction time, reaction temperature,the quantity of catalyst and the quantity of solvent on the reaction results were also studied by orthogonal test and the optimum conditions was obtained as follows: n(itaconic acid)∶n(methanol)∶n (acetyl chloride)=1∶3.5∶0.042, the reaction temperature 65 ℃, reaction time 0.5 h. Under above conditions, the yield and purity of the product were 86 % and 97 % respectively. The structures of product and main impurities were determined by GC-MS.