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作 者:程冬冬 刘九梅 CHENG Dongdong;LIU Jiumei(Development Research Institute of Testing and certification technology.JIANGXI General institute of testing and certification,Nanchang Jiangxi 330029,China)
机构地区:[1]江西省检验检测认证总院检测认证技术发展研究院,江西南昌330029
出 处:《江西化工》2025年第1期55-57,共3页Jiangxi Chemical Industry
摘 要:本实验对对氯甲基苯甲酸叔丁酯的合成进行了研究,对氯甲基苯甲酸叔丁酯的合成主要分为两步,第一步合成对氯甲基苯甲酰氯,第二步对氯甲基苯甲酰氯和叔丁醇钠反应生成对氯甲基苯甲酸叔丁酯,两步反应的产品收率≥94.6%,纯度≥98.4%。实验对合成对氯甲基苯甲酰氯反应中的物料配比、温度、时间、溶剂等因素对反应收率的影响进行了探索,找到了该步反应的最优工艺条件:以甲苯为溶剂,DMF为催化剂,反应温度80℃,物料配比(n_(氯化亚砜):n_(对氯甲基苯甲酸))=1.25。This experiment studied the synthesis of t-butyl chloromethylbenzoate.The synthesis of t-butyl chloromethylbenzoate was mainly divided into two steps.The first step was to synthesize p-chloromethylbenzoyl chloride,and the effects of factors such as material ratio,temperature,time,and solvent on the reaction yield in the synthesis of p-chloromethylbenzoyl chloride were explored.The optimal process conditions for this step were found:toluene as the solvent and DMF as the catalyst,The reaction temperature is 80℃,and the material ratio(n sulfoxide chloride:n p-chloromethylbenzoic acid)is 1.25.The second step is the reaction between chloromethylbenzoyl chloride and sodium tert butanol to generate tert butyl p-chloromethylbenzoate.The yield of the product obtained from the two-step reaction is≥94.6%,and the purity is≥98.4%.
关 键 词:对氯甲基苯甲酸叔丁酯 对氯甲基苯甲酰氯
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