文献类型：期刊文献

中文题名：本芴醇的合成工艺改进

英文题名：Improvement of the Synthesis Process of Benfluoreno

作者：Yang, Kang[1]; Zheng, Qun[1]; Wu, Weiting[1]; Chen, Xuxiang[1]; Zhao, Jianhong[1]

机构：[1] Engineering Research Center of Pharmaceutical Process Chemistry, Ministry of Education, School of Pharmacy, East China University of Science and Technology, Shanghai, 200237, China

年份：2024

卷号：55

期号：8

起止页码：1089

外文期刊名：Chinese Journal of Pharmaceuticals

收录：EI(收录号：20255219800528)

语种：中文

外文关键词：Amination - Chlorination - Chlorine compounds - Drug products - Low temperature production - Process engineering - Reduction

摘要：Using fluorene(2) as the starting material, it was chlorinated by trichloroisocyanuric acid to obtain 2,7-dichlorofluorene(3), which was acylated with chloroacetyl chloride to produce 2,7-dichlorofluorene-4-chloroethyl ketone(4). Then, α-(di-n-butylaminomethyl)-2,7-dichloro-4-fluorenylmethanol(5) was obtained via reduction, cyclization and amination by one-pot method. Finally, 5 was condensed with p-chlorobenzaldehyde to obtain benfluorenol(1), with an overall yield of 36％ and a purity of 99.4％. The improved process used trichloroisocyanuric acid as the chlorinating agent, which improved the selectivity and safety of the reaction. The reduction, cyclization and amination were completed by one-pot method, which reduced the reaction temperature, shortened the reaction cycle, improved production efficiency, and increased the yield from 60％ to 80％. The improved process was simple to operate, low in production cost and suitable for industrial production. ? 2024, Shanghai Institute of Pharmaceutical Industry. All rights reserved.