[关键词]
[摘要]
目的 设计并合成了溴甲纳曲酮在光照、氧化及碱性条件下的3个降解产物。方法 以盐酸纳曲酮为起始原料分别经过500 W紫外灯照射、过氧叔丁醇的三羟甲基氨基甲烷溶液的氧化,氢氧化钠的霍夫曼降解反应得到3个结构不同的降解产物。结果 合成了目标化合物,并利用质谱和核磁数据确证了结构;目标化合物1~3的质量分数分别为99.77%、94.18%、99.51%,收率分别为35.5%、40.0%、25.1%。结论 3个降解杂质的合成与分离为溴甲纳曲酮的杂质研究奠定了物质基础。
[Key word]
[Abstract]
Objective To design and synthesize three degradation products of methylnaltrexone bromide under light, oxidation, and alkaline conditions. Methods Methylnaltrexone bromide was used as raw material to synthesize the three different structure compounds by lighting under 500 W ultraviolet light, oxidation with t-butylhydroperoxide in TRIS solution, Hoffmann degradation with sodium hydroxide. Results The target compounds were synthesized and characterized by MS and NMR data. And the purity detected were 99.77%, 94.18%, and 99.51%, respectively. The yields of three target compounds were 35.5%, 40.0%, and 25.1%. Conclusion The synthesis and separation of three degraded products of methylnaltrexone bromide lay the material base for the study of impurities in methylnaltrexone bromide.
[中图分类号]
[基金项目]