2,6-二甲基-4-苯基-3,5-吡啶二甲酸的合成  

Synthesis of 2,6-Dimethyl-4-phenylpyridine-3,5-dicarboxylic acid

作　　者：谷得发[1] 王伟[1] 刘训帅 朱蕾[1] 孙婷[1] 李公春[1] 

机构地区：[1]许昌学院化学化工学院,河南许昌461000

出　　处：《煤炭与化工》2013年第2期34-35,48,共3页Coal and Chemical Industry

基　　金：河南省高等教育教学改革研究项目(2012SJGLX248);河南省科技计划项目(122102210426);河南省教育厅自然科学研究项目(2011A150025)

摘　　要：为了制备2,6-二甲基-4-苯基-3,5-吡啶二甲酸,首先采取Hantzsch合成法,以0.10 mol苯甲醛、0.125 mol碳酸氢铵和0.25 mol乙酰乙酸乙酯为原料,在40 mL甲醇溶剂中回流0.5 h,合成了1,4-二氢-2,6-二甲基-4-苯基-3,5-吡啶二甲酸二乙酯,产率为45.9%;取0.01 mol 1,4-二氢-2,6-二甲基-4-苯基-3,5-吡啶二甲酸二乙酯在0.02mmol六水三氯化铁的醋酸水溶液中回流反应1 h进行芳构化合成了2,6-二甲基-4-苯基-3,5-吡啶二甲酸二乙酯,产率为50.2%;最后,2,6-二甲基-4-苯基-3,5-吡啶二甲酸二乙酯进行水解合成目标产物,产率为62.7%。In order to prepare 2,6-dimethyl-4-phenylpyridine-3,5-dicarboxylic acid,firstly,by Hantzsch reaction,diethyl 1,4-dihydro-2,6-dimethyl-4-phenylpyridine-3,5-dicarboxylate was prepared by 0.10 mol benzaldehyde,0.25 mol ethyl acetoacetate and 0.125 mol ammonium bicarbonate,refluxing 0.5 h in the solvent of 40 mL methanol.Under the condition of stirring,the yield was 45.9%.Secondly,0.01 mol diethyl 1,4-dihydro-2,6-dimethyl-4-phenylpyridine-3,5-dicarboxylate and 0.02 mmol ferric chloride hexahydrate was added to the reaction system to form the corresponding aromatization diethyl 2,6-dimethyl-4-phenylpyridine-3,5-dicarboxylate under refluxing condition,the yield was 50.2%.Finally the product was synthesized by hydrolyzation,the yield was 62.7%.

关 键 词：2 6-二甲基-4-苯基-3 5-吡啶二甲酸 合成 Hantzsch反应 

分 类 号：O626.32[理学—有机化学]