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作 者:郑兴莉 杜莹 王军 龚维 陈卓 尹晓刚 ZHENG Xingli;DU Ying;WANG Jun;GONG Wei;CHEN Zhuo;YIN Xiaogang(School of Chemistry and Materials Science,Guizhou Normal University,Guizhou Key Laboratory of Functional Materials Chemistry,Guiyang,Guizhou 550025,China)
机构地区:[1]贵州师范大学化学与材料科学学院,贵州省功能材料化学重点实验室,贵州贵阳550025
出 处:《贵州师范大学学报(自然科学版)》2020年第4期50-55,63,共7页Journal of Guizhou Normal University:Natural Sciences
基 金:贵州省科技厅科技支撑项目(黔科合支撑[2016]4023)。
摘 要:以ZnCl2-水滑石(LDH)为催化剂,芳香醛、尿素、乙酰乙酸乙酯为原料,乙醇做溶剂,"一锅法"常温下反应15 min合成6-甲基-2-氧代-4-苯基-1,2,3,4-四氢嘧啶-5-羧酸乙酯衍生物。通过单因素控制变量法,考察了催化剂种类、溶剂、催化剂用量、反应时间、温度及原料摩尔比对目标产物产率的影响。结果表明:在最优条件ZnCl2-LDH催化剂用量为20%(以尿素质量为标准),超声反应15 min,反应温度为25℃,原料摩尔比n(芳香醛)∶n(尿素)∶n(乙酰乙酸乙酯)=1.2∶1.0∶1.0时,产率为63.8%~91.2%。该催化剂可循环使用,循环3次后,产率仍有87.1%。Hydrotalcite(LDH)/ZnCl 2 was used as catalyst,aromatic aldehyde,urea and ethyl acetoacetate were used as raw materials,ethanol was used as solvent,and 6-methyl-2-oxo-4-benzene Ethyl-1,2,3,4-tetrahydropyrimidine-5-carboxylic acid ethyl ester derivative.was synthesized by one-pot reaction at room temperature for 15 min.The effects of catalyst type,solvent,catalyst dosage,reaction time,temperature and raw material molar ratio on the yield of the target product were investigated by single factor control variable method.The results showed that the optimum condition was ZnCl 2-LDH used as catalyst for 20%(based on urea quality,the same below),ultrasonic reaction for 15 min,reaction temperature was 25℃,molar ratio of raw materials n(aromatic aldehyde)∶n(urea)∶n(acetoacetic acid Ethyl ester)=1.2∶1.0∶1.0.The yield was 63.8%~91.2%.The catalyst was recyclable and the yield was 87.1%after 3 cycles.
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