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机构地区:[1]天津医科大学药学院,天津300070 [2]天津市医药科学研究所,天津300020
出 处:《化学试剂》2010年第6期565-566,569,共3页Chemical Reagents
摘 要:2,6-二氯苯基乙酸酯在无水三氯化铝的催化作用下,经Fries重排制得标题化合物。同时采用正交实验的方法考察了温度、催化剂、时间对收率的影响,得到了标题化合物的最优合成工艺,即催化剂与反应物的投料物质的量比为2∶1,温度为110℃,时间为2.5 h。与现有的合成工艺相比,本工艺操作简便、成本较低,且收率较高,粗品收率达到76.1%。2,6-Dichloro-4-acetylphenol(DCAP) was obtained by the Fries rearrangement of 2,6-dichlorophenylacetate,and the reaction was catalyzed by anhydride aluminum chloride.Meanwhile,the method of orthogonal experiments was used to test the influence of temperature,catalyst and reaction time on the product yield.The optimum conditions for the synthesis of 2,6-dichloro-4-acetylphenol were as follows:The molar ratio of the catalyst and reactant was 2.0∶1,the reaction temperature was 110 ℃,and the reaction time was 2.5 h.Compared with the existing synthesis process,the improved process was convenient in operation,and the production cost was lower,with the product yield reaching 76.1%.
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