盐酸地芬尼多中间体N-(3-氯丙基)哌啶的合成及其杂质研究

Synthesis and its Impurity Study of Difenidol Hydrochloride Intermediate 1-(3-chloropropyl) Piperidine

为了控制抗眩晕药盐酸地芬尼多的产品质量,以1,3-溴氯丙烷和六氢吡啶为原料合成了其中间体N-(3-氯丙基)哌啶,并用1,3-二溴丙烷代替1,3-溴氯丙烷合成了杂质1,3-二(1-哌啶基)丙烷,并经MS和NMR进行了研究和结构确证。该杂质的合成可作为盐酸地芬尼多中间体质量控制中的杂质对照,从而对杂质进行准确地定量、定性分析。

To perform the quality control of antidinic drug difenidol hydrochloride, its intermediate 1-（3-chloropropyl） piperidine were prepared with 1-bromo-3-chloropropane and six hydrogen pyridine as raw materials, impurity 1,3-Bis（4-piperidyl）propane were synthesized with 1,3-Dibromopropane instead of 1-bromo-3-chloropropane. The structures were confirmed by NMR and MS. This substance can be used as the reference substance of the impurity in the control of difenidol hydrochloride intermediate.