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机构地区:[1]青岛农业大学化学与药学院,山东青岛266109
出 处:《农药》2013年第8期563-564,567,共3页Agrochemicals
基 金:国家自然科学基金资助项目(21072111);山东省自然科学基金(ZR2011BL003);青岛农业大学博士基金(630708)
摘 要:[目的]2,4-滴丁酯属于苯氧羧酸类除草剂,应用广泛且较少产生耐药性,研发2,4-滴丁酯的绿色合成具有重要意义。[方法]2,4-二氯苯氧乙酸与硼酸三丁酯在无溶剂、无催化剂条件下反应,经减压蒸馏分离得到2,4-滴丁酯。[结果]确定了合成2,4-滴丁酯的最佳反应条件:反应温度140℃,硼酸三丁酯与2,4-二氯苯氧乙酸的摩尔比为2∶1,反应时间4 h,在此条件下酯化率达93.7%。[结论]无溶剂无催化剂条件下合成2,4-滴丁酯,绿色环保,收率高,分离方便,具有工业化应用前景。[Aims] 2,4-D butylate, a class of phenoxyl carboxylic acid herbicide, has been used widely and has less resistance development, green synthesis of 2,4-D butylate is of great significance. [Methods] 2,4-D butylate was obtained by reaction of 2,4-dichlorophenoxyacetic acid with tributyl borate under solvent- and catalyst-free conditions, followed by simple vaccum distillation separation. [Results] The optimized conditions for synthesis of 2,4-D butylate were as follows: the reaction temperature was 140 ~C, the mole ratio of tributyl borate to 2,4-dichlorophenoxyacetic acid was 2 : 1, and the reaction time was 4 h. Under this condition, the esterification rate was 93.7%. [Conclusions] A green and environmentally friendly synthetic route for 2,4-D butylate has been developed in the absence of any solvent and catalyst, which has advantage of high yield, easy separation and highly promising industrial application potential.
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