1-氯甲基-1,2,4-三唑盐酸盐的合成  

Synthesis of 1-(chloromethyl)-1,2,4-triazole hydrochloride salt

作　　者：来虎钦[1] 曾庆斌[1] 丁成荣[1] 周瑛[1] 李万梅[1] 周颖[1] 

机构地区：[1]浙江工业大学化工与材料学院,浙江杭州310032

出　　处：《浙江工业大学学报》2004年第5期569-572,共4页Journal of Zhejiang University of Technology

摘　　要：1-氯甲基-1,2,4-三唑盐酸盐是合成三唑类农药的一个重要中间体。以1H-1,2,4-三唑,多聚甲醛,氯化亚砜为原料经过羟甲基化、氯化反应得到1-氯甲基-1,2,4-三唑盐酸盐。该研究对文献报导的方法进行了探索和改进。实验发现,在合成1-羟甲基-1,2,4-三唑时,不必采用溶剂,在催化剂三乙胺的存在下,1H-1,2,4-三唑与多聚甲醛直接反应结果理想。在合成1-氯甲基-1,2,4-三唑盐酸盐时,先采用适当溶剂如三氯甲烷溶解1-羟甲基-1,2,4-三唑,然后向其中缓慢滴加氯化亚砜。采用该方法明显降低了氯化亚砜的挥发,减少了原料损失,使操作条件更温和,并提高了反应收率。合成总收率达92.3%。1-(chloromethyl)-1,2,4-triazole hydrochloride salt is an important intermediate for preparing pesticides. 1H-1,2,4-triazole was hydroxymethylated with paraformaldehyde in the presence of catalyst. 1-(Hydroxymethyl)-1,2,4-triazole was reacted with thioyl chloride to give 1-(chloromethyl)-1,2,4-triazole hydrochloride salt. In the process of preparation for 1-(hydroxymethyl)-1,2,4-triazole, no solvent is used in the experiment. In the synthesis of 1-(chloromethyl)-1,2,4-triazole hydrochloride salt, a appropriate solvent eg. chloroform is used to dissolve 1-(hydroxymethyl)-1,2,4-triazole, then thioyl chloride is dropped into it. It make the reaction more easy to control and reduce the wastage of thioyl chloride. Total yield was over 92.3%

关 键 词：氯甲基 盐酸盐 1 2 4-三唑 氯化亚砜 合成 羟甲基 多聚甲醛 三乙胺 溶剂 理想 

分 类 号：O626[理学—有机化学] TQ225.241[理学—化学]