以N,N-二甲基甲酰胺作溶剂,2-对甲苯乙炔基苯酚和α-环己烯酮在氯化钯和四丁基碘化铵的作用下,可以顺利发生分子内环化反应一步合成3-(2-对甲苯基苯并呋喃-3-基)环己-2-烯酮。反应最佳条件为:n(2-对甲苯乙炔基苯酚)∶n(α-环己烯酮)∶n...以N,N-二甲基甲酰胺作溶剂,2-对甲苯乙炔基苯酚和α-环己烯酮在氯化钯和四丁基碘化铵的作用下,可以顺利发生分子内环化反应一步合成3-(2-对甲苯基苯并呋喃-3-基)环己-2-烯酮。反应最佳条件为:n(2-对甲苯乙炔基苯酚)∶n(α-环己烯酮)∶n(氯化钯)∶n(四丁基碘化铵)=1∶5∶0.05∶1,反应温度为100℃,反应时间为24h,反应最佳产率82.0%。产物经1 H NMR、13 CNMR和GC-MS确征。展开更多
The synthesis of 3 chloro 2 nitrotoluene using 2,6 dichloroaniline as starting material by diazotization, substitution, condensation, decarboxylic reaction was studied and the best conditions of the synthetic proc...The synthesis of 3 chloro 2 nitrotoluene using 2,6 dichloroaniline as starting material by diazotization, substitution, condensation, decarboxylic reaction was studied and the best conditions of the synthetic procedures were confirmed. Dichloronitrobenzene was obtained in 78.9% yield based on 2,6 dichloroaniline. The reaction of 2,6 dichloronitrobenzene and methyl cyanoacetate with potassium carbonate catalyst in N,N dimethyl formamide gave methyl 2 cyano 2 (3′ chloro 2′ nitrophenyl) acetate in 80.2% yield. The third procedure product 3 chloro 2 nitrophenylacetic acid was obtained by hydrolysis in 82.6% yield. Decarboxylation reaction of 3 chloro 2 nitrophenylacetic acid produced 3 chloro 2 nitrotoluene in 72.9% yield.The structure of products was identified by IR and NMR.展开更多
文摘以N,N-二甲基甲酰胺作溶剂,2-对甲苯乙炔基苯酚和α-环己烯酮在氯化钯和四丁基碘化铵的作用下,可以顺利发生分子内环化反应一步合成3-(2-对甲苯基苯并呋喃-3-基)环己-2-烯酮。反应最佳条件为:n(2-对甲苯乙炔基苯酚)∶n(α-环己烯酮)∶n(氯化钯)∶n(四丁基碘化铵)=1∶5∶0.05∶1,反应温度为100℃,反应时间为24h,反应最佳产率82.0%。产物经1 H NMR、13 CNMR和GC-MS确征。
文摘The synthesis of 3 chloro 2 nitrotoluene using 2,6 dichloroaniline as starting material by diazotization, substitution, condensation, decarboxylic reaction was studied and the best conditions of the synthetic procedures were confirmed. Dichloronitrobenzene was obtained in 78.9% yield based on 2,6 dichloroaniline. The reaction of 2,6 dichloronitrobenzene and methyl cyanoacetate with potassium carbonate catalyst in N,N dimethyl formamide gave methyl 2 cyano 2 (3′ chloro 2′ nitrophenyl) acetate in 80.2% yield. The third procedure product 3 chloro 2 nitrophenylacetic acid was obtained by hydrolysis in 82.6% yield. Decarboxylation reaction of 3 chloro 2 nitrophenylacetic acid produced 3 chloro 2 nitrotoluene in 72.9% yield.The structure of products was identified by IR and NMR.
