合成2-氯吡啶工艺中一个杂质的分析与确定  

Analysis and Confirmation of an Unknown Impurity in a Product of 2-Chloropyridine

作　　者：杨浩 程荣华 龚子扬 张小航 YANG Hao CHENG Rong-hua GONG Zi-yang ZHA NG Xiao-hang(Jiangsu Binhai Economic Development Zone Coastal Industrial Park Administration of Work Safety, Yancheng 224500, China Yancheng Hengsheng Chemical Industrial Co., Ltd., Yancheng 224500, China)

机构地区：[1]江苏滨海经济开发区沿海工业园安全生产监督管理局,江苏盐城224500 [2]盐城恒盛化工有限公司,江苏盐城224500

出　　处：《精细化工中间体》2017年第4期71-73,共3页Fine Chemical Intermediates

摘　　要：对吡啶光催化氯化合成2-氯吡啶过程中产生的主要杂质进行了分析确认。利用HPLC、GC-MS、LC-MS以及~1H NMR确证了该杂质的结构为1-(2-吡啶基)吡啶鎓氯化物,通过实验确定了该杂质的生成条件,并发现少量(5%)水的存在可以有效地抑制此杂质的产生。The impurity produced in the synthesis of 2-chloropyridine was analyzed and speculation. The analytical data from HPLC, LC-MS, GC-MS and 1H NMR indicated that the impurity was [1,2＇-bipyridin]-1-ium chloride. The synthetic experiments suggested the reaction of 2-chloropyridine and pyridine led to the formation of the impurity, which could be largely suppressed by addition of H2O.

关 键 词：2-氯吡啶 1-(2-吡啶基)吡啶翰氯化物 吡啶氯化 

分 类 号：O626[理学—有机化学]