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作 者:宋鹏斌 赵军 SONG Peng-bin;ZHAO Jun(College of Chemistry and Chemical Engineering,Yan'an University,Shaanxi Yan'an 716000,China;College of Environmental Science and Engineering,Tongji University,Shanghai 200092,China)
机构地区:[1]延安大学化学与化工学院,陕西延安716000 [2]同济大学环境科学与工程学院,上海200092
出 处:《当代化工》2019年第11期2521-2524,共4页Contemporary Chemical Industry
摘 要:2,4-二氯苯基丁酮是一种重要的农药、医药中间体,其合成路线包括氧化法、格氏反应、傅克酰基化法等四种路线,存在原料成本高、反应选择性差等问题。傅克酰基化法由于其原料易得,且选择性强是目前合成的主要工艺,但存在收率较低问题。采用傅克酰基化法,以正丁酰氯、间二氯苯、三氯化铝为原料,利用单因素进行了工艺探索,在单因素试验结果基础上利用响应面法对工艺进行了优化,最优条件为:滴加温度=9.3℃,n(正丁酰氯)∶n(间二氯苯)=1.17,n(三氯化铝)∶n(正丁酰氯)=1.11时,产品收率可达69.53%。2,4-Dichlorobenzene butyl ketone is a kind of important pesticide and pharmaceutical intermediate, its synthesis routes include oxidation process, Grignard reaction and Friedel-Crafts acylation.The Friedel-Crafts acetoxylation is the main synthesis process due to its abundant raw materials and good selectivity, but its yield is low. In this paper, by Friedel-Crafts acetoxylation method, 2,4-dichlorobenzene butyl ketone was synthesized from n-butyl chloride and m-dichlorobenzene with aluminium trichloride as catalyst.The process was studied by using single factor experiment. On the basis of single factor experiment results, the process was optimized by using response surface method, the optimal condition was determined as follows: the temperature 9.3℃, n(butyryl chloride):n(m-xylene)=1.17, n(aluminium trichloride):n(butyryl chloride)=1.11.Under above conditions, the product yield reached 69.53%.
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