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微波辐射下不对称1,5-二取代卡巴肼的合成与晶体结构 被引量:4

Microwave-Assisted Synthesis of Asymmetrical 1,5-Disubstituted Carbonohydrazide and Crystal Structure
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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.
出处 《有机化学》 SCIE CAS CSCD 北大核心 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~~
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 asymmetrical 1 5-disubstituted carbonohydrazide synthesis characterization microwave irradiation crystal structure
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