枸橼酸西地那非原料药新的未知杂质的发现与合成

The Discovery dnd Synthesis of New Unknown Impurity in Citrate Sildena

枸橼酸西地那非原料药合成过程中出现的新的未知杂质进行了提纯、结构表征及合成。将氯气通入5-(2-乙氧苯基)-1-甲基-3-丙基-1,6-二氢-7H-吡唑[4,3-d]嘧啶--酮的氯仿溶液中合成杂质-(-氯--乙氧苯基)-1-甲基-3-丙基-1,6-二氢-7H-吡唑[4,3-d]嘧啶-7-酮,并经过LS-MS、NMR、IR确证结构。此杂质未见报道,文献调研及实验研究发现该杂质是造成枸橼酸西地那非原料药纯度降低的主要因素之一,为确保药物安全有效,合成过程中严格控制该杂质的含量。本研究论文侧重于对该杂质形成机理及结构进行表征分析。

The new unknown impurity appeared in the process of the synthesis of sildena citrate was purified,characterized and synthesized.The chlorine gas bubbled into chloroform solution of 5-(2-ethoxyphenyl)-1-methyl-3-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one to synthesis 5-(5-chloro-2-ethoxyphenyl)-1-methyl-3-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one,and the structure were confirmed by MS、NMR、IR.This impurity was not reported that literature researches and experimental studies found that the impurity is one of the main factor to reduce the purity of sildenafil citrate.in order to ensure the drug is safe and effective,strict control of the impurity content in the synthetic process should be taken seriously.This paper focuses on the characterization of the formation mechanism and structure of the impurity.