三氯甲基碳酸酯合成氨基甲酰咪唑的“一锅法”工艺

"One Pot" Techniques for Synthesizing Carbamoylimidazole Using Trichoromethylcarbonate

探讨了由N-[2-(2,4-二氯苯氧基)乙基]丙胺'一锅法'合成1-{N-丙基-N-[2-(2,4-二氯苯氧基)乙基]}氨基甲酰咪唑的工艺条件.结果,适于工业生产的最佳条件是:氯仿作溶剂、胺(1)/三氯甲基碳酸酯/咪唑=1/0.36/1、三氯甲基碳酸酯的浓度为0.37mol/L、滴胺(1)温度为0～40℃、加入咪唑溶液后在氯仿中回流5小时.收率为80%,与逐步法相比(69%×85%)收率提高21%.

The reaction affectors for the synthese of 1 -{ [ N-propyl-N- [ 2- （ 2,4-dichiorophenoxy ） ethyl ] } carbamoylimidazole from N-[2-（2,4-dichiorophenoxy）ethyl] propyl amine in “one pot” way were discussed. The result showed that which used chloroform as solvent,the reactant ratio： amine（ 1 ）/trichloromethyl carbonate/imidazole = 1/0.36/1, the concerntration of trichloromethyl carbonate is 0.37mol/L, reaction temperature dropping amine（ 1 ） is 0 -40℃ and refluxing five hours when imidazole solution had been added in is the best condition for industry prodction. Beaction yield,as 80% , is 21% higher than the step by step way,which is 59%.