碘化钾催化合成4-甲基邻苯二酚二乙酸二甲酯的工艺研究Process Study of KI Catalyzed Synthesis of 4-Methylcatechol Dimethylacetate
杨倩,张雅峥,邵永久,黄少建,罗自萍,董立春
摘要(Abstract)：
以4-甲基邻苯二酚和溴乙酸甲酯为原料,经威廉森缩合反应合成了西瓜酮中间产物4-甲基邻苯二酚二乙酸二甲酯。研究发现适量KI的加入因与溴乙酸甲酯生成活性更高的碘乙酸甲酯可明显提高4-甲基邻苯二酚二乙酸二甲酯的收率,起到了催化剂的作用。研究首先通过熔点测定、NMR、IR和HLPC验证了合成产物的结构和纯度,然后研究了各种反应条件,特别是碘化钾的加入量对4-甲基邻苯二酚二乙酸二甲酯收率的影响,最后采用正交实验确定了反应的最佳条件:KI:C7H8O2(mol:mol)=0.75:1;C3H5BrO2:C7H8O2(mol:mol)=3.5:1;K2CO3:C7H8O2(mol:mol)=4:1;反应时间=6 h;反应温度=80℃。验证实验表明在此条件下4-甲基邻苯二酚二乙酸二甲酯的收率可达到94.7%,而对应的西瓜酮收率可达到67.6%。
关键词(KeyWords)： 4-甲基邻苯二酚二乙酸二甲酯;碘化钾;催化剂;西瓜酮
基金项目(Foundation): 国家自然科学基金(21176270);; 重庆大学研究生创新基金(CDJXS10220013)
作者(Author): 杨倩,张雅峥,邵永久,黄少建,罗自萍,董立春
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