氟喹酮的合成工艺改进

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。

Process Improvement on Synthesis of Afloqualone

Afloqualone was synthesized from isatoic anhydride via seven-step reaction including nitra-tion, reduction, protection, solasodamine, annulation, halogen exchange and deprotection .The struc-ture was confirmed by 1 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 a-gent, toluene, acetonitrile as the solvent , Raney-Ni, TBAB as the catalyst , the total yield can reach 58%, the purity can reach 99%.