盐酸文拉法辛光降解杂质的合成

    Synthesis of Photodegradation Impurities from Venlafaxine Hydrochloride

    • 摘要: 目的 合成盐酸文拉法辛的光降解杂质1-2-(二甲胺基)-1-(4-甲氧苯基)乙烯基-1-环己烷(杂质I),加强对二环类非典型抗抑郁药盐酸文拉法辛原料药的质量控制。方法 对甲氧基苯乙腈与环己酮经缩合反应,LiAlH4还原反应,甲酸/甲醛双甲基化反应得到光降解杂质I。结果 杂质I的结构经1H-NMR、13C-NMR和MS确证,纯度经HPLC检测>99.0%。结论 杂质I可作为盐酸文拉法辛原料药质量控制的杂质对照品。

       

      Abstract: OBJECTIVE To perform the quality control of the bicyclic atypical antidepressant venlafaxine hydrochloride bulk medicine, the venlafaxine hydrochloride photodegradable impurities I2-cyclohexylidene-2-(4-methoxyphenyl)-N,Ndimethylethanamine was prepared. METHODS Through condensation reaction of p-methoxyphenylacetonitrile and cyclohexanone, LiAlH4 reduction reaction, formic acid/formaldehyde double methylation reaction, photodegradable impurities I was obtained. RESULTS The structures of impurities I were confirmed by 1H-NMR, 13C-NMR, MS, and the HPLC indicated that the purity of product was higher than 99.0%. CONCLUSION The impurities I can be used as impurity reference for quality control of venlafaxine hydrochloride active pharmaceutical ingredient.

       

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