摘要
1-甲基-3-乙基-5-吡唑酸乙酯是杀螨剂吡螨胺的重要中间体.探讨了Knorr环合法制备1-甲基-3-乙基-5吡唑酸乙酯的工艺;合成丙酰丙酮酸乙酯中,对反应温度和反应溶剂进行了优化试验,发现用乙醚作溶剂在5℃以下时,反应收率和中间体含量分别达到90%和95%以上.制备1-甲基-3-乙基-5吡唑酸乙酯中,对反应温度和甲基肼与丙酰丙酮酸乙酯的摩尔比进行了优化试验,发现在0℃以下,摩尔比在1∶1.2以上时,目标产物的含量和收率达到95%和85%以上.产品结构经MS,1HNMR,IR表征.
<Abstrcat> Ethyl, 3-ethyl-1-methyl-5-pyrazolecarboxylate synthesized by means of Knorr Reaction is an important intermediate of tebufenpyrad. After the optimized test of temperature and solvent, ethyl propionylpyruvate was produced in ethy1 ether at 5 ℃ of a yield above 90%. The product content is above 95%. Ethyl, 3-ethyl-1-methyl-5-pyrazolecarboxylate was produced of a yield above 85% and product content above 95% with the molar ratio above 1∶1.2 at 0 ℃, after the optimized test of temperature and the molar ratio between ethyl propionylpyruvate and methylhydrazine. The product was characterized by MS,()~1HNMR, IR.
出处
《浙江工业大学学报》
CAS
2005年第3期331-333,共3页
Journal of Zhejiang University of Technology
基金
浙江省教育厅基金资助项目(20030145)
