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作 者:杨翠凤[1] 刘文[2] 林双政[1] 王月梅[1] 陈涛[1] 徐泽刚[1] 王安勇[1]
机构地区:[1]西安近代化学研究所,陕西西安710065 [2]西安建筑科技大学理学院,陕西西安710055
出 处:《精细化工中间体》2015年第3期24-26,共3页Fine Chemical Intermediates
摘 要:提出了一种简便有效的2,2-二氯甲基亚胺酯的合成方法。在室温条件下,以碳酸钾为催化剂,2,2-二氯乙腈为原料制备了2,2-二氯甲基亚胺甲酯和2,2-二氯甲基亚胺乙酯;通过对碱的种类、碱的用量、反应温度和物料比的筛选,确定了反应优化工艺条件:以5%(n/n)的碳酸钾为催化剂,反应物料比为n(2,2-二氯乙腈)∶n(甲醇)=1∶5,在25℃时反应2.5 h。产品收率达95%,纯度>95%。This article reported a improved process for the traditional preparation of 2,2-dichloro methyl imidate.A high efficient method was developed to synthesize two fine chemical intermediates (methyl 2,2- dichloroacetimidate and ethyl 2,2-dichloroacetimidate) at room temperature, and potassium carbonate as a cheaper and easy to obtain chemical was used as the catalyst. In order to obtain the optimum reaction conditions, the influence of the kind of base, the dosage of base, the temperature, and the ratio of the reactants on the reaction was evaluated. The optimum reaction conditions were as following: 2,2-dichloro-acetonitrile (I equiv.) and methanol (5 equiv.) ; reaction time of 2.5 hours; reaction temperature of 25%; potassium carbonate (5 mol%) as the catalyst.
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