以二氯甲烷为溶剂对乙酰基二茂铁Mannich反应的研究  

Mannich reaction of acetylferrocene using dichloromethane as solvent

作　　者：张俊祥[1,2] 高松平[1,2] 周激[2] 

机构地区：[1]中北大学山西省超重力化工工程技术研究中心,山西太原030051 [2]太原工业学院应用化学系,山西太原030008

出　　处：《化学工程》2009年第7期34-37,71,共5页Chemical Engineering(China)

基　　金：山西高校科技研究开发项目(20071515)

摘　　要：利用乙酰基二茂铁的活性α-H的性质进行了乙酰基二茂铁Mannich反应研究,先以磷酸为催化剂,醋酐为酰化剂合成了乙酰基二茂铁,然后探讨在二氯甲烷为溶剂的情况下,乙酰基二茂铁与二乙胺、甲醛的Mannich反应。考察了反应温度、物料摩尔比和反应时间及催化剂的用量对反应条件的影响,并通过红外、质谱对产物进行了表征。确定了以二氯甲烷为溶剂乙酰基二茂铁Mannich反应的合成工艺:乙酰基二茂铁、甲醛、二乙胺的摩尔比为1.0∶2.0∶3.0;操作方式为先加入二乙胺和甲醛,10 min后滴加体积分数为36%盐酸调解pH值在4—6之间,20min后滴加乙酰基二茂铁的二氯甲烷溶液,控制反应温度为50—52℃,反应7 h,产率为77%。Mannich reaction of acetylferrocene was researched by using active α-H nature. Acetylferrocene was synthesized by using acetic anhydride as acetylizing agent and phosphor acid as catalyst. Mannich reaction of acetylferrocene with diethylamine and methanal was discussed using dichloromethane as solvent. The influence of the reaction temperature, mole ratio of the reactants, the reaction time and the quantity of catalyst on the synthetic technology was investigated. The final product was characterized by infrared spectrum （IR） and mass spectrograph （MS）. The synthesis technology for Mannich reaction of acetylferrocene was determined using dichloromethane as solvent. The mole ratios of acetylferrocene, methanal and diethylamine were 1.0 ： 2.0 ： 3.0; the sequence of operation was as follows： first adding methanal and diethylamine, then adding dropwise hydrochloric acid with volume fraction 36% after 10 min to adjust pH between 4-6, adding dropwise dichloromethane solution of acetylferrocene after 20 min, with the reaction temperature of 50-52 ℃ and reaction time of 7 h, the production yield was 77 %.

关 键 词：乙酰基二茂铁 二氯甲烷 MANNICH反应 

分 类 号：O627.81[理学—有机化学]