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作 者:董娴 王琳琳 陈卓 尹晓刚 DONG Xian;WANG Lin-lin;CHEN Zhuo;YIN Xiao-gang(Key Laboratory of Functional Materials Chemistry of Guizhou Province,School of Chemistry and Materials Science,Guizhou Normal University,Guiyang 550001,China)
机构地区:[1]贵州师范大学化学与材料科学学院贵州省功能材料化学重点实验室
出 处:《合成化学》2019年第7期559-562,575,共5页Chinese Journal of Synthetic Chemistry
基 金:贵州省科技厅科技支撑项目(黔科合支撑[2016]2311)
摘 要:以蒙脱土负载路易斯酸为催化剂,催化邻苯二胺和酮经缩合反应合成5个1,5-苯二氮杂卓衍生物,其结构经^1H NMR和IR确证。并对反应条件进行优化了优化。最优反应条件为:n(邻苯二胺)∶n(苯乙酮)=1.0∶2.5,MMT/NiCl210mol%为催化剂,正己烷为溶剂,于70℃反应10h,收率最高为93.0%。Five 1,5-benzodiazepine derivatives were synthesized catalyzed by montmorillonite loaded Lewis acid, using o -phenylenediamine and ketone as raw materials. The structures were confirmed by ^1 H NMR and IR. The reaction conditions were optimized. The results showed that the optimal conditions were as follows: n ( o -phenylenediamine)∶ n (acetophenone)=1.0 ∶ 2.5, 10 mol% MMT/NiCl 2 as the catalyst, n -hexane as solvent, reaction at 70 ℃ for 10 h, the yield was up to 93.0%.
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