摘要
根据1,2,4-噁二唑类化合物的结构特点,采用以苯甲腈为起始原料,经过肟化反应、环合反应、氯代反应和溴代反应四步化学反应合成了5-溴-3-苯基-1,2,4-噁二唑,在合成路线中,前三步反应通过常规的合成方法合成中间产物,第四步溴代反应的反应条件是微波辐射;并对涉及微波反应的工艺条件进行了优化,目标产物及重要中间体的结构经核磁共振波谱和质谱进行了表征。结果表明:当微波功率为200 W,反应温度为150℃,反应时间为15 min时,收率可以达到78.2%,总收率为60.0%。
Accordingto the structuralcharacteristics of1, 2, 4-oxadiazole compounds, 5-bromo-3-phenyl-1, 2, 4-oxadiazole was prepared from benzonitrile through oximation, cyclization, chlorination and bromination. In the synthesis route, the intermediates of the first three steps reaction were synthesized by the conventional methods, and the bromination reaction conditions of the forth step was microwave radiation. The technological parameters involved in microwave reaction were optimized, the structures of the target compound and the intermediates were confirmed by 1 H NMR and MS. The results showed that 5-chloro-3-phenyl-1, 2, 4-oxadiazole reactes with trimethylsilyl bromide under 200 W microwave power, 150℃ for 15 min to give the title compound in 78.2%, and the total yield of the product was 60.0%.
作者
张伟亮
梁芳慧
岳琳
张文英
余同林
王娟
Zhang Weiliang;Liang Fanghui;Yue Lin;Zhang Wenying;Yu Tonglin;Wang Juan(North China Pharmaceutical Corporation Ltd.,Shijiazhuang 052165,China;Shijiazhuang Chemical Fiber Technology Innovation Center of Shijiazhuang University,Shijiazhuang 050035,China)
出处
《煤炭与化工》
CAS
2020年第8期121-123,127,共4页
Coal and Chemical Industry
基金
河北省重点研发计划项目(19211203D)
石家庄市化学纤维技术创新中心建设项目(198190167A)
石家庄市科技型中小企业技术创新基金(19SCX05002)。
