摘要
以4-乙酰氧基苯甲酸甲酯为原料,经无溶剂的Fries重排法合成了3-乙酰基-4-羟基苯甲酸,并对其结构进行了表征。采用L9(34)正交实验,考察了物料投料比、反应温度和反应时间等参数对目标产物收率的影响,并对重排反应机理进行了探讨。结果表明,3-乙酰基-4-羟基苯甲酸的最佳合成工艺为:n(4-乙酰氧基苯甲酸甲酯)∶n(无水三氯化铝)=1∶3、反应温度170℃、反应时间2 h,在此条件下,产物收率达95%。
3-Acetyl-4-hydroxybenzoic acid was synthesized by solvent-free Fries rearrangement method with methyl 4-acetoxybenzoate as a raw material,and the structure of title product was characterized.The effect of feeding ratio,reaction temperature and reaction time on the yield of target product was investigated by L9(34)orthogonal experiment.The mechanism of rearrangement reaction is discussed.The results show that the optimal synthetic conditions are as follows:the ratio of methyl 4-acetoxybenzoate to anhydrous aluminum trichloride is 1∶3,under the reaction temperature of 170℃and the reaction time of 2 h with the yield of 95%.
作者
张茂风
俞颖洁
单春伟
杨沁宜
姚琳琳
Zhang Maofeng;Yu Yingjie;Shan Chunwei;Yang Qinyi;Yao Linlin(College of Pharmacy, Taizhou Polytechnic College, Taizhou 225300, Jiangsu, China;Jiangsu Intelligent Pharmaceutical Industry-Education Integration Center, Taizhou 225300, Jiangsu, China)
出处
《精细石油化工》
CAS
2021年第1期44-47,共4页
Speciality Petrochemicals
基金
江苏省自然科学基金(BK20190246)
江苏省高校自然科学研究项目(19KJB350011)
泰州职业技术学院科研项目(TZYKY-18-30)。
