β-衣康酸单甲酯功能单体的合成

Synthesis of β-methylhydrogen itaconate

以衣康酸和无水甲醇为原料，在酸性催化条件下酯化合成β-衣康酸单甲酯。研究催化剂种类与用量、物料配比、反应温度、反应时间对β-衣康酸单甲酯收率的影响。得到的较佳合成工艺条件为：n（衣康酸）：n（甲醇）：n（苯甲酰氯）=1：3．5：0．043（摩尔比），反应温度65℃，反应时间30min。粗产品用苯和石油醚的混合溶剂重结晶后，产物收率高达97．8％。采用FT-IR和^1H-NMR对产物结构进行了表征。

β-methylhydrogen itaconate was synthesized by using itaconic acid and methyl alcohol as raw materials and using acidic catalyst. The effects of kinds and quantity of catalysts, molar ratio of reactants, reaction time on the reaction were studied. The optimum conditions were obtained as follows： n（itaconic acid）：n（methanol ）：n（benzoyl chloride）= 1：3.5：0.043 （molar ratio）, reaction temperature 65 ℃, reaction time 30 min, The crude product was recrystallized from benzene and petroleum ether. Under above conditions, the yield of the product was 97.8%, The structure of the titled compound was determined by fourier-transferred infrared spectrum（FT-IR） and ^1H-NMR.