摘要
目的 优化雷西莫特的合成工艺.方法 以邻硝基苯甲酸为原料,经还原、缩合、脱水环合、氯代、取代、还原、酰胺化、取代、脱水环合、N-氧代、氨化共10步反应得到目标化合物雷西莫特.结果与结论 目标化合物结构经ESI-MS、1H-NMR和13C-NMR谱确证,总收率为28.6％(以邻硝基苯甲酸计),纯度达99.82％(HPLC法).该工艺原料廉价易得、条件温和、操作简单、适合放大生产.
Abstract
In this study,the synthetic processs of resiquimod was improved.The target compound resiquimod was obtained via ten steps recations,including reduction,condensation,dehydration cyclization,chlorination,substitution,reduction,amidation,substitution,dehydration cyclization,N-oxidation and ammonification,with a total yield of 28.6％and a purity of 99.82％(HPLC).The structure of the target compound was confirmed by ESI-MS,1H-NMR and 13C-NMR.The improved process has the advantages of mild reaction conditions,reduced cost and convenient reaction operation,and is suitable for scale-up production.
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