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机构地区:[1]湖北师范学院化学与环境工程系,湖北黄石435000
出 处:《精细化工中间体》2005年第3期11-12,27,共3页Fine Chemical Intermediates
摘 要:以苯甲腈、叠氮钠、溴等为原料,经偶合,溴化合成了1-溴-5-苯基四氮唑。研究了反应时间、反应温度、溶剂与反应物配比对产品收率的影响。实验表明:在n(苯甲腈)∶n(叠氮钠)=1∶1.1,1 mol NH4Cl催化,120℃下反应20 h可得到收率90%的5-苯基四氮唑。在n(5-苯基四氮唑)∶n(溴)∶n(氢氧化钠)=1∶0.97∶0.96,反应4 h,水作溶剂的条件下,可得到56.4%的1-溴-5-苯基四氮唑,两步反应后的总收率为49.1%。The product 1-Bromine -5-phenyl-tetrazole was synthesized from benzonitrile,Br_(2) and sodium azide by cyclization and bromization. The factors influencing the synthesis were discussed and the best reaction conditions were found out. The optimum conditions were as follow: molar ratio of benzonitrile to sodium azide was 1∶1.1, the catalyst adding was 1.0 mol NH_(4)Cl, the reaction temperature was 120 ℃, and reaction time was 20h, the yield of 5Phenyl-Tetrazole reached 90%; Molar ratio of 5-Phenyl-Tetrazole to sodium hydroxide and bromine was 1∶0.96∶0.97, reaction time 4h and water as solvent, the yield of 1-bromo-5-phenyltetrazole reached 56.4%. The total yield of 1-bromine -5-phenyl-tetrazole could reach 49.1% after cyclization and bromization.
关 键 词:1-溴-5-苯基-四氮唑 5-苯基-四氮唑 合成
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