摘要
以5-溴烟酸（Ⅰ）为起始原料，经SOCl2氯化制备5-溴烟酰氯（Ⅱ），收率为90％；Ⅱ与氨水在冰水浴（0～10℃）下反应合成了5-溴-烟酰胺（Ⅲ），收率为79％；以三氯氧磷为氧化剂，在110％回流反应，将Ⅲ氧化制备成目标产物5-溴烟腈（Ⅳ），收率为68％。以此方法制备5-溴烟腈（Ⅳ）总收率可达到48％。中间产物和目标产物通过傅里叶变换红外光谱和核磁共振氢谱进行了结构确证。
Firstly, 5-Bromo-nicotinic acid, the initial reactant, was chlorinated with SOC12, thus preparing 5 -Bromo-nicofinatc with 90% yield; secondly, 5-Bromo-nicotinamide was prepared from the reaction of 5-Bromo -nieotinate with ammonium aqueous at 0 - 10 ℃ with 79% yield; thirdly, with POC13 as the oxidant, 5-Bromo- nicotinonitrile was obtained by 5-Bromo-nicotinamide via a reflux reaction at 110 ℃ with 68% yield. The total yield was more than 48% by this method. The structures of intermediates and target product were characterized with FT-IR and ^1HNMR.
出处
《辽东学院学报（自然科学版）》
CAS
2010年第1期5-7,共3页
Journal of Eastern Liaoning University:Natural Science Edition
关键词
5-溴烟腈
5-溴烟酸
5-溴烟酰胺
合成
5-Bromo-nicotinonitrile
5-Bromo-nicotinic acid
5-Bromo-nicotinamide
synthesis
