水合肼还原制备3-氨基-2-[(2'-氰基联苯-4-基)甲基]氨基-苯甲酸乙酯的工艺研究

Synthesis technology of ethyl 3-amino-2-[(2'-cyanobiphenyl-4-yl) methylamino]benzoate by hydrazine hydrate reduction method

目的研究3-氨基-2-[(2'-氰基联苯-4-基)甲基]氨基-苯甲酸乙酯的最优合成工艺。方法以2-[(2'-氰基联苯-4-基)-甲基]氨基-3-硝基苯甲酸乙酯为原料,水合肼为还原剂,Pb/C为催化剂,还原制得。结果原料与还原剂的最佳物质的量比为1.92:1,催化剂Pd/C为1.2g,反应温度为75℃,反应时间2h的最优条件下,收率为92.0%。结论本合成工艺稳定,条件温和,产率高,适合3-氨基-2-[(2'-氰基联苯-4-基)甲基]氨基-苯甲酸乙酯的工业化生产。

Objective To optimize the synthesis technology of ethyl 3-amino-2-[（2＇-cyanobiphenyl-4-yl） methylamino] benzoate. Methods Using ethyl 2-[（2＇-cyanobiphenyl-4-yl） methylamino]-3-nitrobenzoate as starting material, hydrazine hydrate as reducing agent, and Pb/C as catalyst, ethyl 3-amino-2-[（2＇-cyanobiphenyl-4-yl） methylamino] benzoate was obtained. Results Under the optimum conditions： molar ratio of raw material-reducing agent was 1.92：1, the quantity of catalyst Pb/C was 1.2 g, and at 75 ℃ for 2 h, the yield reached 92.0%. Conclusion The synthesis technology of ethyl 3-amino-2-[（2＇-cyanobiphenyl-4-yl） methylamino] benzoate is stable, simple, high yield, and could be applied to industry production.