摘要
以三聚氯氰为起始原料,与间二甲苯和间苯二酚在氯化铝和浓盐酸的催化作用下经两次傅克反应一锅法合成了4-[4,6-二(2,4-二甲苯基)-1,3,5-三嗪-2-基]-1,3-苯二醇,产物结构经^(1)H NMR、^(13)C NMR和ESI-MS进行了确证。采用单因素实验考察了催化剂种类、助催化剂用量、反应温度和反应时间对该反应的影响。实验结果表明,较佳的反应条件为:以氯化铝为催化剂,浓盐酸用量为氯化铝质量的6%、第一步反应温度为5℃,第二步反应温度为80℃,4-[4,6-二(2,4-二甲苯基)-1,3,5-三嗪-2-基]-1,3-苯二醇的收率可达91.5%,纯度为99.3%。
4-[4,6-Bis(2,4-dimethylphenyl)-1,3,5-triazin-2-yl]-1,3-benzenediol was synthesized by the one-pot method through Friedel-Crafts reactions using cyanuric chloride,m-xylene,and resorcinol as starting materials in the presence of aluminum chloride and concentrated hydrochloric acid as the catalysts.The structure of the product is confirmed by ^(1)H NMR,^(13)C NMR and ESI-MS.The effects of catalyst type,cocatalyst dosage,reaction temperature and reaction time on the reaction were investigated by single-factor experiments.The experimental results showed that when the catalyst is aluminum chloride,the concentrated hydrochloric acid dosage is 6%of the aluminum chloride mass,the reaction temperature of the first step is 5℃,the reaction temperature of second step is 80℃,the best yield of the 4-[4,6-2(2,4-xylene)-1,3,5-triazine-2-base]-1,3-benzadiol product is 91.5%.The purity of the product measured by HPLC is 99.3%.
作者
丁成荣
韩哲
吴坤
殷燕龙
游兆镭
张国富
Ding Chengrong;Han Zhe;Wu Kun;Yin Yanlong;You Zhaolei;Zhang Guofu(College of Chemical Engineering,Zhejiang University of Technology,Hangzhou 310014,Zhejiang,China)
出处
《精细石油化工》
CAS
2023年第3期30-33,共4页
Speciality Petrochemicals
