3-乙酰氨基邻苯二甲酸酐的合成
Synthesis of N-(1,3-dioxo-1,3-dihydrobenzofuran-4-yl)acetamide
谢月红 1周季颖 1汪锦娟1
作者信息
- 1. 南京医科大学附属南京医院(南京市第一医院)药学部,江苏南京 210000
- 折叠
摘要
3-乙酰氨基邻苯二甲酸酐是合成阿普斯特的关键中间体,以3-硝基邻苯二甲酸为起始原料,经环合、硝基还原、乙酰化制得,并对合成工艺进行了优化.优化条件下目标化合物总收率79.9％(以3-硝基邻苯二甲酸计),纯度98.9％(HPLC),目标化合物结构经ESI-MS、1H NMR表征确证.制备方法操作简便,反应条件温和,所用起始物料及相关试剂便宜易得,可用于工业化生产.
Abstract
N-(1,3-dioxo-l,3-dihydrobenzofuran-4-yl)acetamide,the key intermediate of Apremilast was prepared from 3-nitrophthalic acid via cyclization,reduction,and acetylation.The reaction conditions were optimized for the synthesis of N-(1,3-dioxo-1,3-dihydrobenzofuran-4-yl)acetamide.The total yield of the target compound was improved to 79.9％with the purity of 98.9％(HPLC),and the structure of target compound was identified by ESI-MS and 1H NMR.The improved process is facile and suitable for industrial production with relatively convenient operation procedures,and easily available raw material.
关键词
阿普斯特/3-硝基邻苯二甲酸/合成Key words
Apremilast/3-nitrophthalic acid/synthesis引用本文复制引用
出版年
2024
NETL
NSTL
万方数据