Atapalkar Ranjit S, Kulkarni Amol A
Chemical Engineering & Process Development, CSIR-National Chemical Laboratory Pune, 411008, India.
Academy of Scientific and Innovative Research (AcSIR), Ghaziabad, 201002, India.
Chem Commun (Camb). 2023 Jul 25;59(60):9231-9234. doi: 10.1039/d3cc02402d.
A simple and efficient solvent-free protocol for continuous flow synthesis of amides at room temperature is developed using easily available starting materials. -(3-Dimethylaminopropyl)-'-ethylcarbodiimide hydrochloride (EDC.HCl) was used as the reagent for the formation of an amide bond without using any metal catalyst or additives. A jacketed screw reactor when operated over a residence time of 30 300 s helped achieve almost complete conversion. This approach is extended for the synthesis of 36 derivatives and 2 bioactive molecules using different substrates having different aliphatic mono and di-acids as well as aromatic acids, including aromatic hetero-acid compounds and phenyl hydrazine. The target amide was scaled up to 100 g with an average 90% yield.
利用易得的起始原料，开发了一种简单高效的无溶剂室温连续流合成酰胺的方法。使用1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐（EDC·HCl）作为形成酰胺键的试剂，无需使用任何金属催化剂或添加剂。当夹套式螺杆反应器在30至300秒的停留时间内运行时，有助于实现几乎完全转化。该方法扩展到使用具有不同脂肪族一元和二元酸以及芳香酸（包括芳香杂酸化合物和苯肼）的不同底物合成36种衍生物和2种生物活性分子。目标酰胺放大至100 g，平均产率为90%。
