超声波辅助合成色酮-3-甲酸  

Ultrasonic assisted synthesis of chromone 3-carboxylic acid

作　　者：褚朝森[1] 闫秀美 王晓丽[1] 刘云 李天雪[1] CHU Chao-sen;YAN Xiu-mei;WANG Xiao-li;LIU Yun;LI Tian-xue(Lianyungang TCM Branch of Jiangsu Union Technical Institute,Lianyungang 222007,China;Jiangsu Deyuan Pharmaceutical Co.,Ltd.,Lianyungang 222047,China;Lianyungang Lushui Qingshan Environmental testing Co.,Ltd,Lianyungang 222062,China)

机构地区：[1]江苏联合职业技术学院连云港中医药分院,江苏连云港222007 [2]江苏德源药业股份有限公司,江苏连云港222047 [3]连云港绿水青山环境检测有限公司,江苏连云港222062

出　　处：《化学研究与应用》2024年第8期1935-1940,共6页Chemical Research and Application

基　　金：江苏省连云港市第六期“521工程”新医药科研资助项目(LYG06521202140)资助。

摘　　要：以苯酚为原料,经傅克酰基化、甲酰化、水解三步反应制备了色酮-3-甲酸,总收率57.4%,产物纯度98.6%。甲酰化反应以3-(2-羟基苯基)-3-氧代丙酸甲酯0.05 mol为模型,考察了不同溶剂、甲酸钠用量、超声频率、超声功率、反应温度、反应时间的影响。研究结果表明最优化的反应条件为四氢呋喃作溶剂、甲酸钠与3-(2-羟基苯基)-3-氧代丙酸甲酯的用量摩尔比为1.5:1、超声频率50 kHz、超声功率550 W、温度60℃、反应11 h,该步反应收率为80.0%。Using phenol as starting material,chromone 3-carboxylic acid was prepared by a three-step reaction of Friedel-Crafts acylation,formylation and hydrolysis.The total yield was 57.4%and the purity of the product was 98.6%.In the formylation reaction,taking 0.05 mol methyl 3-(2-hydroxyphenyl)-3-oxopropanoate as research object,effect of solvent type,sodium formate dosage,ultrasonic frequency,ultrasonic power,reaction temperature and time was studied.The result showed that the optimum reaction condition was as follows:using tetrahydrofuran as solvent,mole ratio of sodium formate and methyl 3-(2-hydroxy phenyl)-3-oxopropanoate1.5:1,ultrasonic frequency 50 kHz,ultrasonic power 550W,reaction temperature 60℃,reaction time 11 h,and the yield of this reaction was 80.0%.

关 键 词：色酮-3-甲酸 超声波 甲酰化 

分 类 号：O629.9[理学—有机化学]