绿色肟化反应的综合实验设计  

Design on the Comprehensive Experiment for the Green Oximation Reaction

作　　者：范士明[1] 余伟 李傲齐 董思凡 韩天佼 FAN Shiming;YU Wei;LI Aoqi;DONG Sifan;HAN Tianjiao(State Key Laboratory Breeding Base-Hebei Province Key Laboratory of Molecular Chemistry for Drug,Hebei University of Science and Technology,Shijiazhuang 050018,China;R&D Center,Hebei Grand Jiufu Biotechnology Co.,Ltd.,Baoding 072150,China;New Preparation Branch Factory,North China Pharmaceutical Co.,Ltd.,Shijiazhuang 050000,China)

机构地区：[1]河北科技大学省部共建国家重点实验室培育基地-河北省药用分子化学实验室,石家庄050018 [2]河北远大九孚生物科技有限公司研发中心,保定072150 [3]华北制药股份有限公司新制剂分厂,石家庄050000

出　　处：《实验科学与技术》2024年第2期76-80,共5页Experiment Science and Technology

基　　金：国家自然科学基金(21978068);河北省自然科学基金(H2020208030);河北科技大学研究生课程思政项目(1200769)。

摘　　要：根据科研成果,针对传统肟化反应中存在的问题设计了一种绿色肟化反应的综合实验,对所用的碱和反应装置进行了改进。首先利用湿法研磨制备可循环利用的高活性纳米碳酸钾,通过激光粒径分布仪,扫描电子显微镜(SEM),CO_(2)-程序升温实验(CO_(2)-TPD)进行表征;然后利用纳米碳酸钾为碱合成α-羟亚胺芳基丙酸酯,通过串联装置实现亚硝酸酯的制备与苄基丙二酸二乙酯的肟化反应同步进行。实验避免了醇钠不能回收、腐蚀设备的缺点,解决了亚硝酸酯易挥发造成的贮存、转运困难、容易污染环境的问题。该综合实验利于学生建立环境友好的绿色化学的理念,提高学生综合能力和素质,培养科研创新思维能力。According to some research achievements,a green oximation comprehensive experiment was designed to overcome the shortcomings of the traditional oximation reaction,and the base and reaction equipment were improved.Recyclable nano-K2CO3 was prepared firstly by ultrafine wet milling and characterized by the laser particle size analyzer,scanning electronic microscopy(SEM),and CO_(2)-TPD.The synthesis of ethylα-(hydroxyimino)benzenepropanoate was performed using nano-K_(2)CO_(3)as the base.The preparation of ethyl nitrite and oximation of diethyl benzylmalonate were carried out simultaneously by series devices.The experiment avoids the shortcomings of sodium alkoxides that cannot be recovered and corrodes equipment,and solves the problems of storage and transportation difficulties and easy environmental pollution of volatile nitrite.This comprehensive experiment is beneficial for students to learn the idea of environment-friendly green chemistry,improve the students’comprehensive ability and quality,and cultivate their scientific research innovation thinking ability.

关 键 词：纳米颗粒 绿色化学 肟化反应 碳酸钾 综合实验 

分 类 号：R914.5[医药卫生—药物化学]