摘要
以茶碱和溴代烷为原料,合成了中间体7-烷基咖啡因。在硝酸银催化和过硫酸钾氧化作用下,7-烷基咖啡因与α-羰基酸发生自由基取代反应,得到4种8-酰基咖啡因类似物,并对其结构进行了表征。考察了催化剂用量、氧化剂用量、溶剂体系、反应温度等因素对产品收率的影响,优化反应条件为:催化剂硝酸银的用量为20%、n(7-丁基咖啡因)∶n(过硫酸钾)=1.0∶2.0、反应溶剂为乙腈/水、反应温度100℃。优化条件下,目标化合物1的总收率为54.5%~59.2%。
1,3-Dimethyl-7-alkylxanthine was prepared from theophylline and alkyl bromide. Using AgNO3 as catalyst and K2S2Os as oxidant, 8-substituted acyl caffeine analogues were synthesized via free radical reaction between 1,3- dimethyl-7-alkylxanthine and α-oxo carboxylic acid. Their structures were characterized using ^1H NMR and ^13C NMR. The factors influencing the yield of the reaction were studied. The optimum reaction conditions were as following： the amount of catalyst of 20%, 1.0：2.0 as the ratio ofn （7-butyl caffeine）/n （KES2O8）, a mixture of CH3CN and H2O as reaction solvent and reaction temperature of 100℃. The total yield of the target product was up to 54.5%-59.2%.
作者
郭胜利
李志成
孙纲春
GUO Sheng-li;LI Zhi-cheng;SUN Gang-chun(College of Chemistry, Chemical and Environmental Engineering, Henan University of Techonology, Zhengzhou 450001, China)
出处
《精细化工中间体》
CAS
2018年第1期35-37,48,共4页
Fine Chemical Intermediates
基金
国家自然科学基金项目(21302042)
河南省科技攻关计划项目(162102210040)
