2-(1H-1,2,4-三唑-1-基)乙酰胺的制备

以甲苯作带水剂,三氮唑和氢氧化钾水溶液反应制备三氮唑钾盐;以氯乙酸甲酯和甲胺为原料制备2-氯乙酰甲胺。再以乙腈为溶剂,使三氮唑钾盐和2-氯乙酰甲胺反应制备目的产物2-(1H-1,2,4-三唑-1-基)乙酰胺。着重考察了三氮唑钾盐和2-氯乙酰甲胺反应的反应温度、反应时间及其摩尔比对目的产物收率的影响。从而确定了2-(1H-1,2,4-三唑-1-基)乙酰胺的合成工艺条件为:在乙腈中回流反应,反应时间4 h,n(三氮唑钾盐)∶n(2-氯乙酰甲胺)=1.3∶1;在此条件下,2-(1H-1,2,4-三唑-1-基)乙酰胺的收率达87.5%。并用1H NMR,MS,IR,元素分析对其结构进行了表征。

Synthesis of 2-(1H-1,2,4-Triazol-1-yl)Acetamide

1,2,4-Triazole potassium salt was prepared from 1,2,4-triazole and potassium hydrate using toluene as the water-carrying agent.Then using acetonitrile as the solvent,2-(1H-1,2,4-triazol-l-yl) acetamide was synthesized from 1,2,4-triazole potassium salt and 2-chloro-N-methylacetamide,which was prepared from methyl 2-chloroacetate and methylamine.The effects of reaction temperature,reaction time and molar ratio of materials on preparation of 2-(1H-1,2,4-triazol-1-yl) acetamide from 1,2,4-triazole potassium salt and 2-chloro-N-methylacetamide were investigated.The optimal reaction conditions were obtained as follows: reaction temperature around 80 ℃,reaction time 4 h,n(1,2,4-triazole potassium salt)∶n(2-chloro-N-methylamine)=1.3∶1.The yield of 2-(1H-1,2,4-triazol-l-yl) acetamide was(87.5%.) The product was characterized by ~1H NMR,MS,IR and elemental analysis.