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%.
作者
仲芯颖
褚朝森
李天雪
王晓丽
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)
出处
《当代化工》
CAS
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)
作者简介
仲芯颖(1985-),女,江苏省连云港市人,讲师,2006年毕业于中国药科大学中药资源与开发专业,研究方向:药物研究与分析。E-mail:63083839@qq.com;通讯作者:褚朝森(1982-),男,副教授,硕士,研究方向:生物有机合成。E-mail:chuchaosen@126.com。
