| 引用本文: | 蔡冉,王浦海,张根元.双氯芬酸l-薄荷酯的合成与结构鉴定[J].中国现代应用药学,2015,32(9):1084-1086. |
| CAI Ran,WANG Puhai,ZHANG Genyuan.Synthesis and Characterization of l-Menthyl Diclofenacate[J].Chin J Mod Appl Pharm(中国现代应用药学),2015,32(9):1084-1086. |
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| 摘要: |
| 目的 合成双氯芬酸钠凝胶剂中的杂质——双氯芬酸l-薄荷酯(化合物3)，作为凝胶剂有关物质控制的对照品。方法 双氯芬酸钠(化合物1)经稀盐酸酸化得双氯芬酸(化合物2)；将化合物2以EDCI为脱水剂，DMAP为催化剂，与l-薄荷醇发生酯化反应制得化合物3。结果与结论 目标化合物3的结构经IR、1H-NMR和HR-MS(ESI)谱确证，纯度为99.60%。 |
| 关键词: 双氯芬酸钠 l-薄荷醇 凝胶 双氯芬酸l-薄荷酯 杂质 合成 |
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| Synthesis and Characterization of l-Menthyl Diclofenacate |
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CAI Ran1, WANG Puhai2, ZHANG Genyuan2
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1.Nanjing Tech University, School of Pharmaceutical Sciences, Nanjing 211816, China;2.Nanjing Tech University, Jiangsu Institute of Materia Medica, Nanjing 211816, China
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| Abstract: |
| OBJECTIVE To synthesize l-menthyl diclofenacate (Compound 3), an impurity in diclofenac sodium gel, as a reference substance for the quality control of the gel. METHODS Diclofenac acid (Compound 2) was prepared by acidification of diclofenac sodium with dilute hydrochloric acid (Compound 1). l-Menthyl diclofenacate (3) was synthesized by straightforward esterification of Compound 2 with l-menthol using EDCI as the dehydrator and DMAP as the catalyst. RESULTS & CONCLUSION The structure of the title Compound 3 was confirmed by IR, 1H-NMR and HR-MS(ESI). The purity was about 99.60% as judged by HPLC. |
| Key words: diclofenac sodium l-menthol gel l-menthyl diclofenacate impurity synthesis |
