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作 者:刘长春[1]
机构地区:[1]江苏食品职业技术学院生物化工系,江苏淮安223003
出 处:《化学试剂》2008年第5期375-378,共4页Chemical Reagents
基 金:淮安市科技发展计划项目(HAG03040)资助
摘 要:研究了以TiO2负载Pd-Fe作催化剂,间硝基三氟甲苯常压加氢制备间三氟甲基苯胺,探讨了反应时间、溶剂及其用量、反应温度和催化剂用量等因素对加氢反应的影响,用元素分析、IR和1HNMR对产物的结构进行了表征。优化反应条件为:催化剂用量为2·6g/mol硝基物,无水乙醇作溶剂,用量为0·8L/mol硝基物,反应温度为50℃,0·1MPa下加氢反应2h,产率97·7%,目标产物的纯度达99·2%,催化剂可以重复使用10次。The hydrogenation of m-nitrotrifluorotoluene was studied over TiO2 supported Pd-Fe catalyst at normal pressure. The effects of reaction conditions such as reaction time, amount of solvent, reaetion temperature and amount of eatalyst were investigated. The structure of product was characterized by IR, ^1HNMR spectra and elemental analysis. The optimum conditions of catalytic hydrogenation were as follows : 2.6 g of catalyst was used on one mol of m-nitrotrifluorotoluene,80 mL of ethanol was used on one mol of m-nitrotrifluorotoluene, the reaetion temperature was 50 ℃ ,and the reaction time was 2 h.The yield was 97.7% , the selectivity of m-trifluoromethylaniline was 99.2%.
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