N-glycinylmaleamic acid(GMA) was synthesized by using maleic anhydride and glycine.Five synthesis methods for N-glycinylmaleimide(GMI)were compared.Among them the method using triethylamine to dehydrate was found to b...N-glycinylmaleamic acid(GMA) was synthesized by using maleic anhydride and glycine.Five synthesis methods for N-glycinylmaleimide(GMI)were compared.Among them the method using triethylamine to dehydrate was found to be the best.Their structures were confirmed by fourier transform infrared spectroscopy(FTIR) and nuclear magnetic resonance spectrum(HNMR).展开更多
在低温和碱性条件下,将甘氨酸与碳酸二叔丁酯反应制得N-(叔丁氧羰基)甘氨酸化合物(1).再将化合物1在N,N’-二环己基碳化二亚胺和4-二甲氨基吡啶的作用下与三氟乙胺盐酸盐进行酰胺化制得N-[2-氧代-2-[(2,2,2-三氟乙基)氨基]乙基]氨基甲酸...在低温和碱性条件下,将甘氨酸与碳酸二叔丁酯反应制得N-(叔丁氧羰基)甘氨酸化合物(1).再将化合物1在N,N’-二环己基碳化二亚胺和4-二甲氨基吡啶的作用下与三氟乙胺盐酸盐进行酰胺化制得N-[2-氧代-2-[(2,2,2-三氟乙基)氨基]乙基]氨基甲酸-1,1-二甲基乙酯(2).然后将化合物2在盐酸作用下脱除保护基Boc,得到2-氨基-N-(2,2,2-三氟乙基)乙酰胺.最后通入氯化氢气体制成2-氨基-N-(2,2,2-三氟乙基)乙酰胺盐酸盐(3).化合物1~3经MS、IR、1 H NMR和13 C NMR等确证结构.文中所采用的方法具有原料易得、操作简便、安全性高等优点.展开更多
文摘N-glycinylmaleamic acid(GMA) was synthesized by using maleic anhydride and glycine.Five synthesis methods for N-glycinylmaleimide(GMI)were compared.Among them the method using triethylamine to dehydrate was found to be the best.Their structures were confirmed by fourier transform infrared spectroscopy(FTIR) and nuclear magnetic resonance spectrum(HNMR).
文摘在低温和碱性条件下,将甘氨酸与碳酸二叔丁酯反应制得N-(叔丁氧羰基)甘氨酸化合物(1).再将化合物1在N,N’-二环己基碳化二亚胺和4-二甲氨基吡啶的作用下与三氟乙胺盐酸盐进行酰胺化制得N-[2-氧代-2-[(2,2,2-三氟乙基)氨基]乙基]氨基甲酸-1,1-二甲基乙酯(2).然后将化合物2在盐酸作用下脱除保护基Boc,得到2-氨基-N-(2,2,2-三氟乙基)乙酰胺.最后通入氯化氢气体制成2-氨基-N-(2,2,2-三氟乙基)乙酰胺盐酸盐(3).化合物1~3经MS、IR、1 H NMR和13 C NMR等确证结构.文中所采用的方法具有原料易得、操作简便、安全性高等优点.
