3-硝基-7-二乙氨基香豆素的合成研究
Studies on the Synthesis of 3-Nitro-7-diethylaminocoumarin
刘杰 1梁齐瑞 1李硕 1袁贞祥 1李辰昊 1郭函娟 1张震 1魏标 1陈水生1
作者信息
- 1. 阜阳师范大学化学与材料工程学院,安徽阜阳 236037
- 折叠
摘要
在正丁醇中,以4-二乙氨基水杨醛与硝基乙酸乙酯为原料,通过Knoevenagel缩合反应合成了 3-硝基-7-二乙氨基香豆素,其结构经1HNMR、元素分析及晶体结构表征.研究了该反应的催化剂选择、催化剂用量、原料配比以及助催化剂的用量四个因素对3-硝基-7-二乙氨基香豆素收率的影响,所得最佳合成条件为:催化剂二甲胺摩尔分数为30％,二甲胺与助催化剂冰醋酸1∶1.5(V∶V),4-二乙氨基水杨醛与硝基乙酸乙酯物质的量的比为1∶3,反应时间12 h,3-硝基-7-二乙氨基香豆素收率为89.3％.
Abstract
3-Nitro-7-diethylamino coumarin was synthesized by Knoevenagel condensation of 4-diethylaminosalicylaldehyde with ethyl nitroacetate in n-butanol.The structure was characterized by 1H NMR,elementary analysis and X-ray diffraction analysis.The effects of catalyst selection,amount of catalyst,ratio of raw materials and amount of cocatalyst on the yield were systematically studied.The optimum synthesis conditions were as follows:the molar ratio of dimethylamine catalyst is 30％,the ratio of dimethylamine to cocatalyst glacial acetic acid is 1∶1.5(V∶V),the molar ratio of 4-diethylaminosalicylaldehyde to ethyl nitroacetate is 1∶3,reaction time is 12 h,the yield is 89.3％.
关键词
4-二乙氨基水杨醛/丙二酸二乙酯/二甲胺/3-硝基-7-二乙氨基香豆素Key words
4-diethylaminosalicylaldehyde/diethyl malonate/dimethylamine/3-nitro-7-diethylaminocouma-rin引用本文复制引用
基金项目
教育部产学合作协同育人项目(202101052045)
省级课程思政示范课程建设项目(2020szsfkc0688)
校级线上线下一流课程建设项目(2020HEYL02)
国家级大学生创新创业训练计划(202110371010)
国家级大学生创新创业训练计划(202110371006)
省级大学生创新创业训练计划(S202010371057)
省级大学生创新创业训练计划(S202010371065)
出版年
2024
NETL
NSTL
维普
万方数据