【摘要】 [目的]利用超声波辐射技术合成香豆素-3-甲酸乙酯,并优化其反应条件。[方法]采用超声波辐射技术,经Knoevenagel缩合反应合成了香豆素-3-甲酸乙酯,产物经IR1、HNMR表征。通过单因素优选法研究了不同水杨醛和丙二酸二乙酯投料比例、反应温度、辐射时间、无水乙醇用量、六氢吡啶用量对反应产率的影响。[结果]超声波辐射法制备香豆素-3-甲酸乙酯的最佳合成条件:水杨醛与丙二酸二乙酯物质的量之比为1.001∶.30,无水乙醇25 ml,六氢吡啶0.5 ml,在65℃下,超声波辐射作用80 min,产率达97.46%。[结论]与传统法相比,该合成方法缩短了反应时间,较常规方法产率提高了近20个百分点。更多还原

【Abstract】 [Objective] To synthesize the coumarin-3-carboxylic acid ethyl ester under ultrasonic wave,and optimize its reaction condition.[Method] Coumarin-3-carboxylic acid ethyl ester was synthesized by Knoevenagel condensation reaction of salicylaldehyde and diethyl malonate under ultrasonic wave radiation.The product was characterized through 1HNMR and IR.Single-factor experiments were carried out to study the effect of salicylaldehyde-diethyl malonate ratio,reaction temperature,radiation time,dosage of absolute ethyl alcohol and piperidine on the reaction yield.[Result] The best synthesis conditions of coumarin-3-carboxylic acid ethyl ester under ultrasonic wave were showed as follows: n(salicylaldehyd)∶ n(diethyl malonate)= 1.00∶ 1.30,absolute ethyl alcohol 25 ml,piperidine 0.5 ml,reaction temperature 65 ℃,radiation time 80 min;The yield under these conditions reached 97.46%.[Conclusion] Compared with conventional methods,the reaction time was shortened,and the yield rate increased 20 percentage points under the best condition of ultrasonic wave radiation method.更多还原