色酮-3-甲酸的合成工艺研究  

Research on Synthesis of Chromone 3-Carboxylic Acid

作　　者：仲芯颖[1] 褚朝森[1,2] 李天雪 王晓丽[1] 胡玉涛 ZHONG Xin-ying;CHU Chao-sen;LI Tian-xue;WANG Xiao-li;HU Yu-Tao(Lianyungang TCM Branch of Jiangsu Union Technical Institute,Lianyungang 222007,China;Lianyungang Common Technological Center for Drug Research and Development,Lianyungang 222007,China)

机构地区：[1]江苏联合职业技术学院连云港中医药分院,连云港222007 [2]连云港市药物研发共性技术中心,连云港222007

出　　处：《当代化工》2020年第11期2423-2426,共4页Contemporary Chemical Industry

基　　金：连云港市“521”人才基金项目(项目编号:2017-2019)

摘　　要：以色酮-3-甲醛为原料制备色酮-3-甲腈,后经氢氧化钾水解制备色酮-3-甲酸。考察不同溶剂、氢氧化钾用量、氢氧化钾浓度、温度、时间对水解反应的影响。结果表明,最佳反应条件为:乙二醇做溶剂、氢氧化钾与色酮-3-甲腈物质的量比为5∶1、氢氧化钾浓度为9.7 mol·L-1、反应温度120℃、反应时间5 h,在上述条件下水解反应收率为90%。两步反应总收率为70%。产物经高效液相色谱检测,纯度为98.17%。Using chromone-3-carboxaldehyde as starting material,3-cyanochromone was prepared.Chromone 3-carboxylic acid was synthesized via hydrolysis of 3-cyanochromone by potassium hydroxide.The effect of solvent,potassium hydroxide dosage,potassium hydroxide concentration,temperature,time on hydrolysis reaction was studied.The result showed that the optimum reaction condition was as follows:using ethylene glycol as solvent,mole ratio of potassium hydroxide and 3-cyanochromone 5∶1,potassium hydroxide concentration 9.7 mol·L-1,120℃,reaction time 5 h.Under above conditions,the yield of hydrolysis reaction was 90%.The total yield of the two-step reaction was 70%.The product purity determined by HPLC was 98.17%.

关 键 词：色酮-3-甲酸 色酮-3-甲醛 色酮-3-甲腈 水解 

分 类 号：TQ225.12[化学工程—有机化工]