以4-甲基邻苯二酚为原料,经氧化、酯化两步反应合成产物3,4-二羟基苯甲酸乙酯,并采用IR、1 H NMR和13 C NMR对产物结构进行了表征。通过一系列实验,探讨了催化剂TBAB用量、高锰酸钾用量、反应时间、反应温度对3,4-二羟基苯甲酸产率的影...以4-甲基邻苯二酚为原料,经氧化、酯化两步反应合成产物3,4-二羟基苯甲酸乙酯,并采用IR、1 H NMR和13 C NMR对产物结构进行了表征。通过一系列实验,探讨了催化剂TBAB用量、高锰酸钾用量、反应时间、反应温度对3,4-二羟基苯甲酸产率的影响,以及酯化反应中催化剂TsOH用量、乙醇用量、反应时间和反应温度对3,4-二羟基苯甲酸乙酯产率的影响。在最优合成条件下,3,4-二羟基苯甲酸乙酯的产率可达90.5%。实验证明本合成方法提高了产率,降低了成本,具有较好的工业应用前景。展开更多
4substituted ethyl2methyl6,7methylenedioxy3quinolinecarboxylate was prepared from 3,4methylenedioxy-phenylketones Ⅳ,yield of Ⅳa-Ⅳd is 74～87%.The synthetic route consists of acylation,nitration,...4substituted ethyl2methyl6,7methylenedioxy3quinolinecarboxylate was prepared from 3,4methylenedioxy-phenylketones Ⅳ,yield of Ⅳa-Ⅳd is 74～87%.The synthetic route consists of acylation,nitration,reduction and condensation.Moleculor structures of Ⅳa～Ⅳd were determined by IR,1H NMR and MS.展开更多
通过水代替有机溶剂来提纯2-丙基-4,5-1 H-咪唑二羧酸二乙酯和4-(1-羟基-1-甲基乙基)-2-丙基-1 H-咪唑-5-羧酸乙酯的新方法,使得改进工艺更加绿色简便。采用1 H NMR、13 C NMR、IR、MS谱图对反应后的产品和未知杂质进行结构鉴定,确证为...通过水代替有机溶剂来提纯2-丙基-4,5-1 H-咪唑二羧酸二乙酯和4-(1-羟基-1-甲基乙基)-2-丙基-1 H-咪唑-5-羧酸乙酯的新方法,使得改进工艺更加绿色简便。采用1 H NMR、13 C NMR、IR、MS谱图对反应后的产品和未知杂质进行结构鉴定,确证为一水合4-(1-羟基-1-甲基乙基)-2-丙基-1 H-咪唑-5-羧酸乙酯和4-乙酰基-2-丙基-1 H-咪唑-5-羧酸乙酯。对反应的可能机理进行初步研究。展开更多
A compound ethyl(5S,6R)-2-(4-methylphenyl)-6-[(1R)-tert-butyldimethylsilyloxyethy]-penem-3-carboxylate was synthesized through displacement,acylation and Wittig cyclization reaction of optically active material(3R,4R)...A compound ethyl(5S,6R)-2-(4-methylphenyl)-6-[(1R)-tert-butyldimethylsilyloxyethy]-penem-3-carboxylate was synthesized through displacement,acylation and Wittig cyclization reaction of optically active material(3R,4R)-3-[(1R)-tert-butyldimethylsilyloxyethyl]-4-acetoxy-2-azetidi-none(4AA)upon thionocarboxlic acid.The intermediates and the target product were characterized by 1HNMR,IR,elementary analysis and MS.展开更多
文摘以4-甲基邻苯二酚为原料,经氧化、酯化两步反应合成产物3,4-二羟基苯甲酸乙酯,并采用IR、1 H NMR和13 C NMR对产物结构进行了表征。通过一系列实验,探讨了催化剂TBAB用量、高锰酸钾用量、反应时间、反应温度对3,4-二羟基苯甲酸产率的影响,以及酯化反应中催化剂TsOH用量、乙醇用量、反应时间和反应温度对3,4-二羟基苯甲酸乙酯产率的影响。在最优合成条件下,3,4-二羟基苯甲酸乙酯的产率可达90.5%。实验证明本合成方法提高了产率,降低了成本,具有较好的工业应用前景。
文摘4substituted ethyl2methyl6,7methylenedioxy3quinolinecarboxylate was prepared from 3,4methylenedioxy-phenylketones Ⅳ,yield of Ⅳa-Ⅳd is 74～87%.The synthetic route consists of acylation,nitration,reduction and condensation.Moleculor structures of Ⅳa～Ⅳd were determined by IR,1H NMR and MS.
文摘通过水代替有机溶剂来提纯2-丙基-4,5-1 H-咪唑二羧酸二乙酯和4-(1-羟基-1-甲基乙基)-2-丙基-1 H-咪唑-5-羧酸乙酯的新方法,使得改进工艺更加绿色简便。采用1 H NMR、13 C NMR、IR、MS谱图对反应后的产品和未知杂质进行结构鉴定,确证为一水合4-(1-羟基-1-甲基乙基)-2-丙基-1 H-咪唑-5-羧酸乙酯和4-乙酰基-2-丙基-1 H-咪唑-5-羧酸乙酯。对反应的可能机理进行初步研究。
文摘A compound ethyl(5S,6R)-2-(4-methylphenyl)-6-[(1R)-tert-butyldimethylsilyloxyethy]-penem-3-carboxylate was synthesized through displacement,acylation and Wittig cyclization reaction of optically active material(3R,4R)-3-[(1R)-tert-butyldimethylsilyloxyethyl]-4-acetoxy-2-azetidi-none(4AA)upon thionocarboxlic acid.The intermediates and the target product were characterized by 1HNMR,IR,elementary analysis and MS.
