无溶剂微波辅助一锅法合成吡喃并[2,3-c]吡唑衍生物  

Solvent-free One-pot Synthesis of Pyrano[2,3-c]pyrazole Derivatives under Microwave Irradiation

作　　者：吴璐璐[1] 岳阳 曹占奇 姜松[1] 高萌璐 樊小改 潘振良[1] WU Lu-lu;YUE Yang;CAO Zhan-qi;JIANG Song;GAO Meng-lu;FAN Xiao-gai;PAN Zhen-Hang(College of Science,Henan Agricultural University,Zhengzhou 450002,China)

机构地区：[1]河南农业大学理学院,河南郑州450002

出　　处：《化学试剂》2021年第2期247-252,共6页Chemical Reagents

基　　金：河南农业大学自然科学类青年创新基金项目(KJCX2020A19);河南农业大学本科实验室开放创新项目(KF1917);河南农业大学博士启动基金项目(30601333);大学生创新训练计划项目(2019104660)。

摘　　要：绿色、高效、简便的催化多组分一锅法反应符合当前所倡导的"绿色"化学理念,是当今有机化学的研究热点。通过在无溶剂微波辅助条件下,使用廉价易得的KF/Al_(2)O_(3)催化吡唑啉酮、芳香醛和丙二腈的多组分"一锅法"反应,合成了一系列吡喃并[2,3-c]吡唑衍生物,反应时间为5~10 min,产率为85%~98%。标题化合物的结构经核磁共振波谱(NMR)和高分辨质谱(HR-MS)确证。方法克服了传统合成方法中溶剂对环境造成的污染及分步合成的不便,具有无溶剂参与、反应时间短且产率高的优点。催化剂回收重复使用3次,其催化活性不受影响。The green,efficient and simple catalytic reaction with multi-component one-pot is in line with the current"green"chemical concept,and is now a research hotspot in organic chemistry.KF/Al_(2)O_(3)as a cheap and readily accessible catalyst for the solvent-free synthesis of pyrano[2,3-c]pyrazole derivatives by multi-component one-pot reaction of pyrazolone,aryl aldehydes,malononitrile was described.The reaction time was 5~10 min,the yield ranged from 85%to 98%.The target products were confirmed by nuclear magnetic resonance spectroscopy(NMR)and high resolution mass spectrometry data(HR-MS).Compared with the traditional synthetic methods,the work overcomes the environmental pollution caused by the use of solvent and the inconvenience of stepwise reaction and has the advantages of solvent-free,short reaction time and high yield.The catalyst can be recovered and reused for three cycles without loss of activity.

关 键 词：无溶剂合成 微波辅助合成 一锅法 吡喃并[2 3-c]吡唑衍生物 

分 类 号：O626.32[理学—有机化学]