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作 者:马立强 张伟 MA Li-qiang;ZHANG Wei(Jiyuan Hengshun New Material Co.,Ltd.,Jiyuan 459000,China)
机构地区:[1]济源市恒顺新材料有限公司,河南济源459000
出 处:《化学与粘合》2022年第3期221-223,242,共4页Chemistry and Adhesion
摘 要:以对氟甲苯为原料,经氯化、水解、精馏制备对氟苯甲酰氯。通过对氯化反应、水解反应条件进行筛选,得出最优反应条件:(1)氯化反应时,反应温度为100~105℃,反应时间5h,抑制剂为三乙醇胺,且m(三乙醇胺)∶m(对氟甲苯)=0.7∶1000,在此条件下,反应收率98.5%;(2)水解反应时,反应温度为120℃,催化剂为三氯化铁,且n(三氯化铁)∶n(对氟三氯苄)=0.02∶1,在此条件下,反应收率98.9%。两步总收率高达97.4%。With p-fluorotoluene as raw material,the p-fluorobenzoyl chloride is synthesized through the chlorination,hydrolysis and rectification.By screening the conditions of chlorination reaction and hydrolysis reaction,the optimal reaction conditions are obtained:(1)during the chlorination reaction,when the reaction temperature is 100~105℃,the reaction time is 5h,the inhibitor is triethanolamine,and m(triethanolamine)∶m(p-fluorotoluene)= 0.7∶1000,the reaction yield will be 98.5%;(2)during the hydrolysis reaction,when the reaction temperature is 120℃,the catalyst is ferric chloride,and n(ferric chloride)∶n(p-fluorotrichlorobenzyl)= 0.02∶1,the reaction yield will be 98.9%.The total yield of the two steps is as high as 97.4%.
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