3-氨基-1,3,4,5-四氢-2H-1-苯并氮杂䓬-2-酮的合成

Synthesis of 3-Amino-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one

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-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-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。

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-tetrahydm-2H-l-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% ）.