2-乙氧基苯甲酸的合成新方法  

Synthesis of 2-Ethoxybenzoic Acid

作　　者：刘志超[1] 张晓伟 王刚[1] 张帆[1] 

机构地区：[1]辽宁医学院药学院,辽宁锦州121001 [2]辽宁省计划生育科学研究院药物研究室,辽宁沈阳110031

出　　处：《化学试剂》2015年第12期1143-1145,共3页Chemical Reagents

基　　金：辽宁医学院"校长基金"奥鸿博泽基金医药创新基金项目(XZJJ20130104-04)

摘　　要：采用一种新方法合成西地那非重要中间体标题化合物:以水杨酸甲酯为原料,丙酮为溶剂,在氢氧化钾的存在下与硫酸二乙酯发生乙基化反应,反应完毕蒸除丙酮后,直接在氢氧化钠水溶液中水解生成标题化合物,总收率为94.3%(以水杨酸甲酯计)。通过改变硫酸二乙酯的用量、水杨酸甲酯与氢氧化钾的反应时间、氢氧化钠的用量,得到了标题化合物的优化制备工艺条件。An optimized process for the synthesis of 2-ethoxybenzoic acid was reported,which was a key intermediate for the preparation of sildenafil. As the starting material,methyl salicylate was reacted with diethyl sulfate in the presence of potassium hydroxide in acetone. After the completion of the reaction,the solvent was removed by distillation,followed by a hydrolysis reaction in aqueous sodium hydroxide,and generated 2-ethoxybenzoic acid. The overall yield of the process was 94. 3%,which was calculated by methyl salicylate. The reaction conditions were optimized by changing the amount of diethyl sulfate,reaction time of methyl salicylate and potassium hydroxide as well as the amount of sodium hydroxide.

关 键 词：2-乙氧基苯甲酸 西地那非 合成工艺 

分 类 号：O625[理学—有机化学]