利鲁唑的合成新工艺  

A Novel Synthetic Process for Riluzole

作　　者：鲍广龙 张乃华 张超 焉兆凯 张贵民 BAO Guanglong;ZHANG Naihua;ZHANG Chao;YAN Zhaokai;ZHANG Guimin(National Engineering and Technology Research Center of Chirality Pharmaceutical,Shandong New Time Pharmaceutical Co.,Ltd.,Linyi 273400)

机构地区：[1]国家手性制药工程技术研究中心,山东新时代药业有限公司,山东临沂273400

出　　处：《中国医药工业杂志》2023年第6期881-883,共3页Chinese Journal of Pharmaceuticals

摘　　要：报道了利鲁唑(1)的合成新工艺。以2-氨基-5-(三氟甲氧基)苯硫醇(2)为起始物料,与硫脲(3)在盐酸作用下反应制得1-[2-巯基-4-(三氟甲氧基)苯基]硫脲(4),4经CuSO_(4)·5H_(2)O/三乙胺催化发生分子内环化得目标产物1,纯度99.9%,总收率79.3%(以2计)。该路线未见文献报道,改进后的工艺稳定、操作简便。A novel synthetic process of riluzole(1) was reported in this paper.1-[2-Mercapto-4-(trifluoromethoxy)phenyl]thiourea(4) was prepared through the condensation of 2-amino-5-(trifluoromethoxy)benzenethiol(2) and thiourea(3) in the presence of hydrochloric acid.Then,4 was transformed into the target compound through intramolecular cyclization catalyzed by CuSO_4·5H_2O/TEA system with an overall yield of 79.3%(based on 2) and a purity of 99.9%.This synthetic method with stable process and simple operation has not yet been reported in previous literature.

关 键 词：利鲁唑 肌萎缩性脊髓侧索硬化 合成工艺 

分 类 号：R971[医药卫生—药品] TQ460.6[医药卫生—药学]