摘要
以丁酮和2,4-二硝基苯肼为原料,无水氯化铵为催化剂,在室温下,通过无溶剂研磨法合成丁酮缩2,4-二硝基苯腙。考察了原料摩尔比、研磨时间以及催化剂用量对产率的影响,在单因素实验的基础上进行正交实验,探究出一条高产率的合成工艺,对合成产物进行了紫外光谱表征。实验结果显示:最佳合成工艺为:室温下,2,4-二硝基苯肼的量为0.20 g,原料n(丁酮)∶n(2,4-二硝基苯肼)为1.4∶1,研磨时间为20 min,催化剂用量为15 mmol,产率高达76%。
Butanone 2,4-dinitrophenylhydrazone was synthesized by solvent-free grinding at room temperature with butanone and 2,4-dinitrophenylhydrazine as raw materials and anhydrous ammonium chloride as catalyst.The effects of raw material ratio,grinding time and catalyst dosage on the yield were investigated.On the basis of single factor experiment,an orthogonal experiment was carried out to explore a high yield synthesis route.The melting point and ultraviolet spectra of the synthesized product were characterized.The experimental results show that the optimal synthesis conditions:at room temperature are as follows:the amount of 2,4-dinitrophenylhydrazine is 0.20 g,butanone:2,4-dinitrophenylhydrazine(molar ratio)is 1.4∶1,grinding time is 20 min,catalyst dosage is 15 mmol,the highest yield is 76%.
作者
黄晓雯
李灿津
黎晓桐
冯敏捷
向海均
苏碧森
陈洪
Huang Xiaowen;Li Canjin;Li Xiaotong;Feng Minjie;Xiang Haijun;Su Bisen;Chen Hong(Guangdong Ocean University,Zhanjiang 524088,China)
出处
《山东化工》
CAS
2021年第21期3-5,共3页
Shandong Chemical Industry
基金
2019年广东海洋大学大学生创新创业训练计划项目(CXXL2019309)
广东省2020年度课程思政建设改革示范项目(139)
2020年度广东海洋大学本科教学质量与教学改革工程项目(93)
2020年度广东海洋大学一流本科课程(8)。
关键词
丁酮缩2
4-二硝基苯腙
无溶剂
研磨法
合成
腙类化合物
butanone 2,4-dinitrophenylhydrazone
solvent-free
grinding method
synthesis
hydrazone compounds
