五氯化铌/离子液体[BMIm]Br共催化合成酰胺化合物

Synthesis of amide compounds enabled by niobium pentachloride and ionic liquid [BMIm]Br cooperative catalysis

摘要:

以脂肪族或芳香羧酸和脂肪胺为原料，制备了一系列酰胺类化合物。建立了一种温和条件下五氯化铌和离子液体共同参与的催化脂肪族或芳香羧酸和脂肪胺直接酰胺化方法，用于高效制备酰胺类化合物。对催化剂用量、反应溶剂、反应时间以及反应温度进行了优化。结果表明，在最佳反应条件下（有机酸2.0 mmol，有机胺2.0 mmol，五氯化铌0.16 mmol，1-甲基-3-丁基咪唑溴化物0.3 mmol，4A分子筛200 mg，甲苯4 mL，反应温度110 ℃，反应时间24 h），酰胺收率为77%~96%。

Abstract:

A series of amide compounds have been prepared, using aliphatic or aromatic carboxylic acids and fatty amines as raw materials. A method for the direct amidation of carboxylic acids and amines with the participation of niobium pentachloride and ionic liquids has been established for the efficient preparation of amides. The influencing factors of reaction, such as the amount of catalyst, reaction solvent, reaction time and reaction temperature, were optimized. The results show that the yield of amidation reaction can reach 77-96% under the optimal reaction conditions (organic acid 2.0 mmol, organic amine 2.0 mmol, niobium pentachloride 0.16 mmol, 3-butyl-1-methyl-1H-imidazol-3-ium bromide 0.3 mmol, 4A M.S. 200 mg, toluene 4 mL, reaction temperature 110 oC, reaction time 24 h).