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机构地区:[1]上海石油化工研究院催化四部,上海201208
出 处:《化学世界》2005年第1期34-37,共4页Chemical World
摘 要:以氯代苯腈(2,6 二氯苯腈、2 氯苯腈和4 氯苯腈)和无水氟化钾为原料,非质子极性溶剂(环丁砜、1,3 二甲基2 咪唑啉酮等)为反应介质,经氟化反应合成了相应的氟代苯腈(2,6 二氟苯腈、2 氟苯腈和4 氟苯腈)。得出的最佳合成条件为:n(CBN)∶n(KF)∶n(Solv)∶n(Cat.)=1∶2.5~3.0∶4.5~8.8∶0~0.006,反应温度为230~280°C,反应时间为2.0~4.5h。产品摩尔收率分别为93.5%、91.8%、90.5%,质量分数分别为99.5%、99.1%、99.0%。Fluorobenzonitriles (2,6-DFBN,2-FBN,4-FBN) were prepared by fluorination of chlorobenzonitriles (2,6-DCBN,2-CBN,4-CBN) with potassium fluoride using sulfolane and 1,3-dimethyl-2-imidazolidinone(DMI) as non-polar solvents. The optimum synthetic conditions were as follows: n(CBN)∶n(KF)∶n(Solv)∶n(Cat)=1∶2.5~3.0∶4.5~8.8∶0~0.006;reaction temperature, 230~(280°C); reaction time, 2.0~4.5 h. The yields of 2,6-DFBN, 2-FBN and 4-FBN were (93.5%),91.8% and 90.5% and the purity was 99.5%, 99.1% and 99.0%, respectively.
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