首页|3-硝基-7-二乙氨基香豆素的合成研究

3-硝基-7-二乙氨基香豆素的合成研究

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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％.
Studies on the Synthesis of 3-Nitro-7-diethylaminocoumarin
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％.

4-diethylaminosalicylaldehydediethyl malonatedimethylamine3-nitro-7-diethylaminocouma-rin

刘杰、梁齐瑞、李硕、袁贞祥、李辰昊、郭函娟、张震、魏标、陈水生

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阜阳师范大学化学与材料工程学院,安徽阜阳 236037

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

教育部产学合作协同育人项目省级课程思政示范课程建设项目校级线上线下一流课程建设项目国家级大学生创新创业训练计划国家级大学生创新创业训练计划省级大学生创新创业训练计划省级大学生创新创业训练计划

2021010520452020szsfkc06882020HEYL02202110371010202110371006S202010371057S202010371065

2024

10.19500/j.cnki.0367-6358.20220501

化学世界
上海市化学化工学会

化学世界

影响因子：0.264
ISSN：0367-6358
年,卷(期)：2024.65(1)
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