3-氨基-1,3,4,5-四氢-2H-1-苯并氮杂革-2-酮的合成

摘要

3-Amino-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one in total yield of 90％ was synthesized by aminization reaction of 3-bromo-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one with benzylamine,and then through hydrogenation reaction catalyzed by 5％ Pd/C.The optimum hydrogenation reaction conditions at 100 ℃/2.5 MPa for 10 h were as follows:absolute alcohol was solvent,amount of 5％Pd/C was 10％.The yield of 3 was 95.5％ and the purity was 99.7％ under the optimum reaction conditions.The 5％Pd/C catalyst could be reused for 7 times without change in yield(about 95％).%以3-溴-1,3,4,5-四氢-2H-1-苯并氮杂--2-酮为起始原料,与苄胺反应制得3-苄氨基-1,3,4,5-四氢-2H-1-苯并氮杂(堇)-2-酮(2)；2经5％ Pd/C催化加氢合成了3-氨基-1,3,4,5-四氢-2H-1-苯并氮杂——革)-2-酮(3),总收率90％.最佳氢化反应条件为:以无水乙醇为溶剂,5％ Pd/C用量为总用量的10％,于100℃/2.5 MPa条件下反应10 h,3的收率95.5％,纯度99.7％.5％ Pd/C可套用7次,收率稳定在95％左右.