氟喹酮的合成工艺改进  

Process Improvement on Synthesis of Afloqualone

作　　者：徐盼云 陈志卫[1] 

机构地区：[1]浙江工业大学药学院绿色制药技术与装备教育部重点实验室,浙江杭州310014

出　　处：《合成化学》2016年第9期824-827,共4页Chinese Journal of Synthetic Chemistry

摘　　要：以靛红酸酐为起始原料,经硝化、还原上保护、氨解开环、环合、卤素交换和脱保护共七步反应合成了氟喹酮(7),其结构经1H NMR,13C NMR和ESI-MS确证。研究了硝化试剂、溶剂、催化剂等对7收率的影响,结果表明:在使用浓硝酸作为硝化试剂,甲苯,乙腈等为溶剂,Raney-Ni,TBAB等为催化剂时,总收率可达58%,纯度达99%以上。Afloqualone was synthesized from isatoic anhydride via seven-step reaction including nitration,reduction,protection,solasodamine,annulation,halogen exchange and deprotection. The structure was confirmed by1 H NMR,13 C NMR and ESI-MS. The influence of nitration reagents,solvents,catalysts on the yield of 7 were studied. The results showed that when using nitric acid as nitrating agent,toluene,acetonitrile as the solvent,Raney-Ni,TBAB as the catalyst,the total yield can reach58%,the purity can reach 99%.

关 键 词：肌松药 氟喹酮 靛红酸酐 药物合成 

分 类 号：O621.3[理学—有机化学] R914.5[理学—化学]