香豆素-3-羧酸乙酯的无溶剂微波合成研究  

Synthesis of coumarin-3-ethyl formate under microwave irradiation without solvent

作　　者：徐翠莲[1] 杨楠[2] 刘善宇[2] 杨国玉[1] 王彩霞[1] 苏惠[1] 王喜云[1] 

机构地区：[1]河南农业大学理学院,河南郑州450002 [2]河南农业大学烟草学院,河南郑州450002

出　　处：《河南农业大学学报》2009年第4期468-471,共4页Journal of Henan Agricultural University

基　　金：河南省教育厅基金项目(2009A150012)

摘　　要：以取代水杨醛和丙二酸二乙酯为原料，在微波辐射和无溶剂条件下以六氢吡啶为催化剂发生缩合反应合成了6个香豆素-3-羧酸乙酯，目标化合物的结构均经IR,^1H NMR和^13C NMR进行了表征．利用正交设计探讨了实验的最优工艺条件为：微波功率400W、反应时间6rain、醛与丙二酸二乙酯摩尔比1：1．3和催化荆用量0．3mL．在优化条件下，香豆素-3-羧酸乙酯的产率为39．2％～85．9％．与常规合成方法相比，该优化的合成方法具有反应时间短、产率高、环境友好等特点．Six coumarin-3-ethyl formates were synthesized from substituted salicylaldehyde and diethyl monlonate under microwave irradiation without solvent. The structure of the title compounds were characterized by IR, ^1H NMR and ^13C NMR. The optimum parameters of eoumarin-3-ethyl formate were obtained by orthogonal test ： microwave power 400 W, reaction time 6 min, ratio of aldehyde to diethyl monalate 1 ： 1.3 and piperizine 0.3 mL respectively. Under this optimized condition, the yield of the title compounds were 39.2% -85.9% with such advantages as short time, high yields and environmentally benign procedures compared with the traditional methods.

关 键 词：香豆素-3-羧酸乙酯 微波 合成 无溶剂 正交实验 

分 类 号：O622.5[理学—有机化学]