酸功能化介孔聚合物微波辅助合成3,4-二氢嘧啶-2(1H)- 1

IF 0.9 Q4 CHEMISTRY, MULTIDISCIPLINARY Current Microwave Chemistry Pub Date : 2021-02-01 DOI:10.2174/2213335608666210329130736
Bishwajit Changmai, K. Rajkumari, D. Das, Lalthazuala Rokhum
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引用次数: 0

摘要

研究了酸官能化介孔聚合物催化剂的合成及其在微波辐射下通过Biginelli缩合反应合成3,4-二氢嘧啶-2(1H)-酮的应用。采用FT-IR、BET、TEM、SEM和EDX等分析技术对合成的聚合物催化剂进行了表征。催化剂的高酸度(1.15mmol g-1)、高表面积(90.44m2g-1)和介孔性质有效地促进了3,4-二氢嘧啶-2(1H)-酮的合成。在醛/乙酰乙酸乙酯/尿素摩尔比为1:1:1.2、催化剂负载量为6wt.%(相对于醛)、温度为80°C、微波功率为50W的优化反应条件下,微波辐射显示出比常规加热(15-25%产率)更高的产率(89-98%)。对催化剂的可重复使用性进行了长达5个连续循环的研究,它在合成3,4-二氢嘧啶-2(1H)-酮方面表现出极大的稳定性,而产率没有任何显著下降。
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Microwave-Assisted Synthesis of 3,4-Dihydropyrimidin-2(1H)-Ones Using Acid-Functionalized Mesoporous Polymer
Synthesis and application of acid-functionalized mesoporous polymer catalyst for the synthesis of 3,4-Dihydropyrimidin-2(1H)-ones via Biginelli condensation reaction under microwave irradiation is investigated. Several analytical techniques such as FT-IR, BET, TEM, SEM and EDX were employed to characterize the synthesized polymeric catalyst. High acidity (1.15 mmol g-1 ), high surface area (90.44 m2 g -1 ) and mesoporous nature of the catalyst effectively promoted the synthesis of 3,4-Dihydropyrimidin-2(1H)-ones. Microwave irradiation shows higher yield (89-98 %) as compared to conventional heating (15-25 % yield) under our optimized reaction conditions such as 1:1:1.2 molar ratio of aldehyde/ethylacetoacetate/urea, catalyst loading of 6 wt.% (with respect to aldehyde), the temperature of 80 °C and microwave power of 50 W. The synthesized Biginelli products were fully characterized by 1H and 13C NMR. The reusability of the catalyst was investigated up to 5 successive cycles and it showed great stability towards the synthesis of 3,4-Dihydropyrimidin-2(1H)-ones without any significant depreciation in yields.
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来源期刊
Current Microwave Chemistry
Current Microwave Chemistry CHEMISTRY, MULTIDISCIPLINARY-
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