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出 处:《化学世界》2013年第11期682-684,共3页Chemical World
摘 要:研究了以邻二氯苯为溶剂,以三苯基膦为相转移催化剂,4-氯代苯酐为原料与碱金属盐KF反应制得4-氟苯酐的新工艺。考察了反应温度、催化剂用量、溶剂用量、配料比对4-氟苯酐收率的影响。研究表明,以4-氯代苯酐质量28g为基准,反应温度为190℃,催化剂用量2.24g,溶剂用量为30mL,4-氯代苯酐与无水氟化钾摩尔比1∶3时,4-氟苯酐收率达到97.07%。. 4-Fluorophthalic anhydride was prepared by the reaction of 4-chlorophthalic anhydride with po- tassium fluoride in the presence of a phase transfer catalyst and 1,2-dichlorobenzene as solvent. The effect of reaction conditions, such as reacting time, reaction temperature, ratio of raw materials, amount of cata- lyst and solvent, on the yield of 4-fluorophthalic anhydride was studied. The results showed that the opti- mum conditions were as follows. 28 g 4-chlorophthalic anhydride reacting with 26.73 g KF, amount of tri- phenylphosphine 2.24 g, reaction temperature 190℃, and amount of solvent 30 mL. Under such condi- tions the yield of 4-fluorophthalic anhydride was 97. 07%.
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