“4-吡啶甲基取代的苯并三氮唑”的合成工艺优化

Optimization of Synthetic Technics of "4-picolyl Substituted Benzotriazole"

目的探索并优化4-吡啶甲基取代的苯并三氮唑的目标产物的合成工艺条件。方法以1-H苯并三氮唑和4-氯甲基吡啶盐酸盐为原料、乙酸乙酯为溶剂、无水碳酸钾为缚酸剂,一步合成了标的物,并采用红外吸收光谱,核磁共振谱、质谱进行结构表征。结果苯并三氮唑和氯甲基吡啶盐酸盐直接在无水碳酸钾/乙酸乙酯作为溶剂、缚酸剂,85℃回流4 h,总产率提高到72.36%。结论通过简化亲核取代反应条件,可以直接一步合成目标产物1-[(4-吡啶基)甲基]-苯并三唑(B1)和2-[(4-吡啶基)甲基]-苯并三唑(B2),并大大提高了产率。

Objective Explore the optimum conditions for preparing title product.Methods Title products were directly synthesized with benzotriazole and 4-（chloromethyl） pyridinium chloride with the K2CO3 as acid binging agent in ethyl acetate solvent.The products were characterized by IR,1HNMR and MS.Results The processes of the reaction were simplified and the total yield of title products was improved to 72.36%.Conclusion With one step direct synthesis,the reaction conditions were simplified,and that the yield was increased greatly.