微通道反应器中连续化合成苯亚甲基丙酮——介绍一个大学化学综合实验
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摘要
微反应是近年来化学研究领域发展迅猛的一门新兴技术,本实验以苯甲醛和丙酮作为原料,在氢氧化钠作用下通过缩合反应连续化合成苯亚甲基丙酮。通过对摩尔配比、停留时间、反应温度等影响因素的考查,确定了较佳反应条件,并采用核磁和质谱对产品结构进行表征。与传统的批式方法相比,本实验方案具有收率高、操作简便、实验结果稳定等优点。本实验将先进技术和理念寓于实验教学中,不仅增强了学生的实验技能,而且有助于学生了解科学前沿、研究现状、发展方向和应用前景,激发学生的学习兴趣。
Micro-reaction is an emerging technology that has been developing rapidly in recent years in all research fields of chemistry. In this experiment, benzaldehyde and acetone were used as the starting materials, thus(E)benzalacetone was continuously synthesized by condensation reaction in the presence of sodium hydroxide. By investigating effects of mole ratio, residence time and reaction temperature, the optimized reaction conditions were determined. The product was characterized by NMR and MS. Compared with traditional batch synthetic methods, the presented method has the advantages of high yield, simple operation, and reproducible experimental results. This work gives advanced technology and ideas in laboratory teaching, which not only enhances students' experimental skills, but also helps students to understand the frontiers of science, research situation, tendency of development and application prospects, as well as inspire students' interest greatly.
Micro-reaction is an emerging technology that has been developing rapidly in recent years in all research fields of chemistry. In this experiment, benzaldehyde and acetone were used as the starting materials, thus(E)benzalacetone was continuously synthesized by condensation reaction in the presence of sodium hydroxide. By investigating effects of mole ratio, residence time and reaction temperature, the optimized reaction conditions were determined. The product was characterized by NMR and MS. Compared with traditional batch synthetic methods, the presented method has the advantages of high yield, simple operation, and reproducible experimental results. This work gives advanced technology and ideas in laboratory teaching, which not only enhances students' experimental skills, but also helps students to understand the frontiers of science, research situation, tendency of development and application prospects, as well as inspire students' interest greatly.
引文
[1]张国林,韩莹,薛怀国,刁国旺.大学化学, 2010, 25(1), 23.
[2]庄媛,刘杰民,姚喆.大学化学, 2017, 32(7), 44.
[3]丁养军,刘永军.化学试剂, 1996, 18(2), 119.
[4]Wiles, C.; Watts, P. Micro Reaction Technology in Organic Synthesis, 1st ed.; CRC Press(an imprint of Taylor&Francis Group):Boca Raton,USA, 2011; pp 1–432.
[5]Noda Perez, C.; Perez, C. A.; Henriques, C. A. Appl. Catal. A Gen. 2004, 1–2, 229.
[6]Wang, X. Q.; Saleh, R. Y.; Ozkan, U. S. J. Catal. 2005, 231(1), 20.
[7]Zhu, Y. W. J. Fluorine Chem. 2011, 132(1), 71.
[8]Conard, C. R.; Dolliver, M. A. Org. Synth. 1943, 2, 167.
[9]Tao, H.; Duan, J.; Li, P. Asian J. Org. Chem. 2014, 3, 644.
[10]Daneshfar, Z.; Rostami, A. RSC Advances 2015, 5(127), 104695.
[2]庄媛,刘杰民,姚喆.大学化学, 2017, 32(7), 44.
[3]丁养军,刘永军.化学试剂, 1996, 18(2), 119.
[4]Wiles, C.; Watts, P. Micro Reaction Technology in Organic Synthesis, 1st ed.; CRC Press(an imprint of Taylor&Francis Group):Boca Raton,USA, 2011; pp 1–432.
[5]Noda Perez, C.; Perez, C. A.; Henriques, C. A. Appl. Catal. A Gen. 2004, 1–2, 229.
[6]Wang, X. Q.; Saleh, R. Y.; Ozkan, U. S. J. Catal. 2005, 231(1), 20.
[7]Zhu, Y. W. J. Fluorine Chem. 2011, 132(1), 71.
[8]Conard, C. R.; Dolliver, M. A. Org. Synth. 1943, 2, 167.
[9]Tao, H.; Duan, J.; Li, P. Asian J. Org. Chem. 2014, 3, 644.
[10]Daneshfar, Z.; Rostami, A. RSC Advances 2015, 5(127), 104695.