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作 者:姚转乐[1] 姬明理[1] 王融冰[1] 刘红利[1]
出 处:《应用化工》2009年第9期1283-1285,共3页Applied Chemical Industry
基 金:陕西省科学技术研究发展计划项目(2007XCP-10)
摘 要:以乙二胺、尿素、甲醛和甲酸为原料,经过环化和甲基化反应制得目标产物1,3-二甲基-2-咪唑啉酮(1,3-DMI)。通过红外、核磁对其结构进行了确证。考察了溶剂、原料浓度、原料摩尔比、反应温度和时间、催化剂对制备(1,3-DMI)收率的影响。较佳工艺条件为:制备2.眯唑啉酮时,以水-乙二醇混合作溶剂;制备1,3-DMI时,甲醛(36%):甲酸(85%)摩尔比为1:2.8,反应温度95—100℃,反应时间16h,氯化亚铜和三乙胺作催化剂,用量分别是2-咪唑啉酮摩尔数的1.0%。总收率达到71%,纯度为98.5%。Using ethylenediarnine, urea, methanal and formic acid as base material, 1,3-dimethyl-2-imid- azolidinone was prepared via cyclization reaction and methylation. Its structure was characterized by IR and 1H NMR. The effect of solvent, material concentration, material ratio, reaction temperature and reac- tion time, catalyst on the preparation were studied. The better technology has been obtained:taking water- EG as solvent 2-imidazolidinone was prepared. The molar ratio of the methanal (36%) to the formic acid (85%) is 1:2.8 ,reaction temperature is 95 - 100℃,reaction time is 16 h,taking cuprous chloride and triethylamine as catalyst, the molar ratio of the cuprous chloride and triethylamin to 2-imidazolidinone is 1.0% while 1,3-DMI was prepared. The yield of 1,3-DMI could reach 71% ,the purity of 1,3-DMI is 98.5%.
关 键 词:制备 2-咪唑啉酮 1 3-二甲基-2-咪唑啉酮
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