摘要
以2-吡啶甲酸和乙腈为原料,次氯酸叔丁酯(t-BuOCl)为引发剂,碱为添加剂,通过脱羧偶联反应一步合成N-(2-吡啶)-乙酰胺。分别考察了反应温度、反应时间、次氯酸叔丁酯用量以及碱的种类和用量对反应收率的影响,结果表明:最佳的工艺条件为2-吡啶甲酸0.3 mmol、碳酸钾0.15 mmol、次氯酸叔丁酯0.9 mmol、乙腈3 mL、反应温度60℃、反应时间20 h。在此优化条件下,N-(2-吡啶)-乙酰胺的收率为88%。
N-(pyridin-2-yl)acetamide was synthesized by 2-picolinic acids and acetonitrile as starting materials,t-BuOCl as initiator and base as additives through one-step decarboxylation coupling reaction.The effects of factors including reaction temperature,reaction time,the amount of t-BuOCl and base were investigated.Results showed that the decarboxylative coupling of 2-picolinic acid with acetonitrile were performed in the presence of 2-picolinic acids(0.3 mmol),t-BuOCl(0.9 mmol),K_(2)CO_(3)(0.15 mmol)and acetonitrile(3 mL)at 60℃for 20 h.Under the optimized conditions,the N-(pyridin-2-yl)acetamide was obtained in 88%.
作者
戚明甫
张西涛
仲恩奎
严明
周飞翔
QI Mingfu;ZHANG Xitao;ZHONG Enkui;YAN Ming;ZHOU Feixiang(Jiangsu Yangnong Chemical Group Co.,Ltd.,Yangzhou 225000,China)
出处
《精细石油化工进展》
CAS
2022年第1期20-24,共5页
Advances in Fine Petrochemicals
