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微波辅助“一锅煮”法合成p-羟基肉桂酸
Microwave-assisted “one-pot” synthesis of p-hydroxycinnamic acid
【摘要】 微波辐射下,文章以p-羟基苯甲醛和乙酸酐为原料,碳酸钾为催化剂,经Perkin反应"一锅煮"法合成p-羟基肉桂酸,并优化了反应条件。实验结果表明:在p-羟基苯甲醛、乙酸酐和碳酸钾摩尔比为1∶4∶1,微波辐射功率为700 W,回流反应20min,水解反应2h的条件下,p-羟基肉桂酸的产率达到71.94%,纯度为99.20%。产物结构经傅里叶红外光谱仪(FT-IR)、超导核磁共振波谱仪(1 H NMR)和显微熔点仪分析表征并加以确认。
【Abstract】 P-hydroxycinnamic acid was synthesized from p-hydroxybenzaldehyde,acetic anhydride and potassium carbonate by Perkin reaction under microwave irradiation.The reaction conditions were optimized.The results showed that the maximum yield of p-hydroxycinnamic acid reached 71.94% and the purity of the compound reached 99.20% when the mole ratio of p-hydroxybenzaldehyde,acetic anhydride and potassium carbonate was 1∶4∶1,the microwave radiant power was 700 W,the refluxing reaction time was 20 min and the hydrolysis reaction time was 2h.The structures of the product were identified by Fourier transform infrared spectrometer(FT-IR),superconducting nucleus magnetic resonance spectrometer(1 H NMR)and micro melting point instrument.
【Key words】 p-hydroxybenzaldehyde; potassium carbonate; Perkin reaction; microwave irradiation; "one-pot" method;
- 【文献出处】 合肥工业大学学报(自然科学版) ,Journal of Hefei University of Technology(Natural Science) , 编辑部邮箱 ,2016年10期
- 【分类号】TQ245.4
- 【被引频次】1
- 【下载频次】95