摘要
标题化合物是重要的精细化工中间体,对其合成工艺进行优化。以2-氯烟酸和固体光气为原料,氯化、氨化得到2-氯烟酰胺,2-氯烟酰胺在次氯酸钠溶液和氢氧化钠溶液中霍夫曼酰胺降解得到2-氯-3-氨基吡啶,其经过自由基取代得标题化合物。在优化的反应条件下,收率达75.6%,纯度99%。该法操作简便、适合工业化生产,其化学结构经1HNMR分析得到确证。
2,3-Dichloropyridine is an important fine chemical intermediate, this work aims to optimize and improve the synthetic process. 2-Chloronicotinamide was obtained from 2-chloronicotinic acid and biscarbonate as staring material via the process of chlorination and ammonification. 2-Chloro-3-aninopyridine was prepared by reaction of 2-chloronicotinamide with NaC10 solution and NaOH solution. Finally ,2,3-dichloropyridine was prepared by radical substitution reaction with 2-chloro-3-aninopyridine. Under the optimal conditions,the total yield was 75.6% and the purity was 99% . The synthetic process has simple operation,and is suitable for industrial production. The product was confirmed by ^1HNMR.
出处
《化学试剂》
CAS
北大核心
2016年第9期911-913,916,共4页
Chemical Reagents
关键词
2
3-二氯吡啶
2-氯烟酸
合成
2,3-dichloropyridine
2-chloronicotinic acid
synthesis
