[關(guān)鍵詞]
[摘要]
目的 研究3-氨基-2-[(2'-氰基聯(lián)苯-4-基)甲基]氨基-苯甲酸乙酯的最優(yōu)合成工藝。方法 以2-[(2'-氰基聯(lián)苯-4-基)-甲基]氨基-3-硝基苯甲酸乙酯為原料,水合肼為還原劑,Pb/C為催化劑,還原制得。結(jié)果 原料與還原劑的最佳物質(zhì)的量比為1.92∶1,催化劑Pd/C為1.2 g,反應(yīng)溫度為75 ℃,反應(yīng)時間2 h的最優(yōu)條件下,收率為92.0%。結(jié)論 本合成工藝穩(wěn)定,條件溫和,產(chǎn)率高,適合3-氨基-2-[(2'-氰基聯(lián)苯-4-基)甲基]氨基-苯甲酸乙酯的工業(yè)化生產(chǎn)。
[Key word]
[Abstract]
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.
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