一锅法合成二氢吡啶工艺的优化研究  

Study on optimization of synthesis process of dihydropyridine by one-pot method

作　　者：闵江 梁景乐 刘正光 赵才兵 娄燕 赵腾飞 MIN Jiang;LIANG Jing-le;LIU Zheng-guang;ZHAO Cai-bing;LOU Yan;ZHAO Teng-fei

机构地区：[1]山东胜利生物工程有限公司,山东济宁272000 [2]中牧实业股份有限公司,北京100095

出　　处：《饲料研究》2023年第24期91-93,共3页Feed Research

摘　　要：试验旨在优化一锅法合成二氢吡啶的过程。以乌洛托品、乙酰乙酸乙酯及乙酸铵水溶液为原料,乙醇为溶剂一锅法合成二氢吡啶,通过单因素试验对物料配比、溶剂配比、反应温度、反应时间等因素进行优化。结果显示,二氢吡啶合成的优选参数为n_(乌洛托品)∶n_(乙酰乙酸乙酯)∶n_(醋酸铵)=1∶7∶0.8进行投料,乌洛托品投料量∶溶剂量=1∶3.5~1∶4.5,混合溶剂中水与乙醇占比为V_(水)∶V_(乙醇)=20∶15~30∶15,60℃下反应1.5 h,二氢吡啶含量高达98%~103%,产物收率可达90%左右,母液可循环套用。研究表明,该工艺路线具有低污染、高生产安全性、产率高的优点,是合成二氢吡啶的一种环境友好的工艺路线。The experiment was to optimize the synthesis of dihydropyridine by one-pot method.Dihydropyridine was synthesized from urotropine,ethyl acetoacetate and ammonium acetate aqueous solution with ethanol as the solvent by a one-pot method.The material ratio,solvent ratio,reaction temperature and reaction time were optimized by a single factor test.The results showed that the optimal parameter for the synthesis of dihydropyridine was n_(urotropine)∶n_(acetoacetate)∶n_(ammonium acetate)=1∶7∶0.8 for feeding,the dosage of urotropine and the amount of solvent was 1∶3.5~1∶4.5,and the ratio of water to ethanol in the mixed solvent was V_(water)∶V_(ethanol)=20∶15~30∶15.The reaction was carried out for 1.5 h at 60℃,the content of dihydropyridine was as high as 98%~103%,the product yield could reach 90%,the mother liquor could be recycled.The study indicates that the process has the advantages of low pollution,high production safety and high yield,which is an environmentally friendly route for the synthesis of dihydropyridine.

关 键 词：二氢吡啶 乌洛托品 乙酰乙酸乙酯 饲料添加剂 

分 类 号：S816.7[农业科学—饲料科学]