摘要
为高效、低成本、低污染地合成2-(4-甲基戊基-2-基)-3-氨基噻吩,探索以3-氨基噻吩-2-甲酸甲酯为原料,经乙酰基保护、酯基水解、脱羧、偶联、酰胺水解、加氢还原6步反应合成的新路线.探讨偶联、水解反应的机理,并对各步反应进行优化.结果表明,优化后反应的总收率为78.6%,产物的质量分数为98.1%.该工艺的原料廉价易得、操作简单、反应条件温和,且各步反应溶剂可实现套用,产生的“废水”和“废溶剂”较少,有工业化应用前景.
A new route for the synthesis of 2-(4-methylpentyl-2-yl)-3-aminothiophene from methyl 3-aminothiophene-2-formate by six steps of acetyl protection,ester hydrolysis,decarboxylation,coupling,amide hydrolysis and hydrogenation reduction was developed.The mechanism of coupling and hydrolysis was discussed,and the reaction steps were optimized.After optimization,the total yield of the reaction was 78.6%,and the gas chromatographic content of the product was 98.1%.The raw materials of the process are cheap and easy to obtain,the operation is simple,the reaction conditions are mild,and the reaction solvents in each step can be applied,resulting in less“wastewater”and“waste solvents”,which has a bright future in industrialization.
作者
杜友兴
Du Youxing(Shanghai Chemspec Corporation,Shanghai 200331,China)
出处
《宁夏大学学报(自然科学版)》
CAS
2019年第4期370-374,共5页
Journal of Ningxia University(Natural Science Edition)
基金
普陀区高层次人才科研创新基金资助项目(普人才2014-A-09)