摘要
以碳酸钾为缚酸剂,4 硝基 邻苯二甲酰亚胺与五种卤代试剂在N,N 二甲基甲酰胺(DMF)中回流反应3h,生成相应的N 取代 4 硝基 邻苯二甲酰亚胺(1),产率为46.4%～92.5%.硝基物在盐酸体系40℃下经氯化亚锡还原,得到N 取代 4 氨基 邻苯二甲酰亚胺(2),产率为29.6%～92.2%.氮气保护条件下,2与乙醇在固体光气作用下生成(2 取代 1,3 二酮 2,3 二氢 1H 异吲哚 5 ) 氨基甲酸乙酯(3),3的产率为67%～92%.各化合物的结构均经1H NMR、IR、元素分析和FAB MS证实.
Five N-substituted-4-nitrophthalimides(1)were prepared using 4-nitrophthalimide and the corresponding halogenides as starting materials,and potassium carbonate as activator.4-nitrophthalimide and halogenides were stirred in DMF at reflux temperature for 3 h to give N-substituted-4-nitrophthalimides(1) with yields of 46.4%—92.5%.Reduction of N-substituted-4-nitrophthalimides(1)to the corresponding amines(2)was performed in hydrochloric acid at 40 ℃ using stannous chloride as reduction agent, yielding products of 2 of (29.6%)—92.2% .Under the N_2 atmosphere,(2-substituted-1,3-dioxo-2,3-dihydro-1H-isoindol-5-yl)-carbamic acid ethyl esters(3) were synthesized by 2, triphosgene and ethanol at the rate of 67%—92%.The structures of the products were confirmed by^1H-NMR,IR,elemental analysis and FAB-MS.
出处
《天津大学学报（自然科学与工程技术版）》
EI
CAS
CSCD
北大核心
2004年第5期447-450,共4页
Journal of Tianjin University：Science and Technology
