微波辐射下不对称1,5-二取代卡巴肼的合成与晶体结构  

Microwave-Assisted Synthesis of Asymmetrical 1,5-Disubstituted Carbonohydrazide and Crystal Structure

作　　者：朱继华[1,2] 郑旭东[1,2] 郭国哲[1,2] 张玉全[1,2] 仵博万[1,2] 

机构地区：[1]陇东学院化学化工学院 [2]陇东学院-氟乐邦表面活性中心,庆阳745000

出　　处：《有机化学》2015年第9期1975-1980,共6页Chinese Journal of Organic Chemistry

基　　金：甘肃省自然科学基金(No.1208RJZM289);庆阳市科技局工业支撑重点(No.KZ2014-27)资助项目~~

摘　　要：在水相中,以水杨醛和卡巴肼为原料,室温下高产率合成了1-(2-羟基苯亚甲基)卡巴肼(3),随后以乙醇/冰醋酸为混合溶剂、微波功率为350 W、温度为120℃和其他芳香醛/酮反应16~30 min得到1,5-二取代卡巴肼衍生物4a^4p,并用IR、1H NMR、13C NMR和元素分析对其结构进行了表征.与传统的方法相比,该法具有简单、快速、高效和对环境友好等优点,为不对称双席夫碱的合成提供一定的参考.X射线衍射分析表明化合物4i属于单斜晶系,P21/c空间群.A series of asymmetrical 1,5-disubstituted carbonohydrazides 4a-4p were synthesized by the condensation of various substituted aromatic aldehydes and 1-（2-hydroxyphenylidene）carbonohydrazide（3） under microwave irradiation at 120 ℃ and 350 W in ethanol-sulfuric acid mixture for 16-30 min. The starting materials 3 was synthesized using salicylaldehyde and carbohydrazide under water at room temperature. The new synthesized compounds were characterized by IR, ^1H NMR, ^13C NMR spectra and elemental analysis. Compared with the conventional heating method, this method is simple, fast, efficient and eco-friendly. This reaction is expected to be a powerful tool for the synthesis of asymmetrical Schiff bases compounds. The X-ray diffraction analysis indicates that the compound 4i belongs to monoclinic, space group P21/c.

关 键 词：不对称1 5-二取代卡巴肼 合成 表征 微波辐射 晶体结构 

分 类 号：O625.6[理学—有机化学]