2-氯-5-三氯甲基吡啶的定向合成与结构测定

The Selectively Synthesis and Characterization of 2-Chloro-5-trichloromethylpyridine

利用3-甲基吡啶为原料,通过光氯化反应合成并分离出了2-氯-5-三氯甲基吡啶。探讨了光氯化反应的机理,通过正交实验对其工艺进行优化,得到了合成产物的最佳工艺条件:温度为180℃,时间为10h,原料与溶剂体积比为1∶3,产物产率可达到53.1%。同时用IR、1HNMR、13CNMR、MS、UV-Vis等光谱手段确定了产品的结构。

2-Chloro-5-trichloromethylpyridine was prepared adopting 3-methylpridine as raw material by photochemical chlorination. The mechanism of photochemical chlorination and the reaction conditions affecting yield were studied by the kroenecker method. The optimal conditions with yield of 53.1% are as follows： 10 h of reaction time, 180℃ of reaction temperature, 1：3 of（3-methylpyridine）/（1,2-dichlorobenzene）（by vol）. The structure of product was characterized by ^1HNMR ^13C NMR IR,MS and UV-Vis.