| 丹曲林钠杂质B的合成 |
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| 引用本文： | 周月广,涂增清,罗兰庆,李光州,李合. 丹曲林钠杂质B的合成[J]. 合成化学, 2017, 0(1). DOI: 10.15952/j.cnki.cjsc.1005-1511.2017.01.16189 |
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| 作者姓名： | 周月广 涂增清 罗兰庆 李光州 李合 |
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| 作者单位： | 丽珠集团 丽珠医药研究所,广东 珠海,519020 |
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| 摘 要： | 以5-对硝基苯胺为原料,与糠醛经重氮化反应制得5-对硝基苯基糠醛(1);1与1-氨基乙内酰脲盐酸盐经缩合、精制得丹曲林(2);2与甲醇钠成盐制得丹曲林钠(3);3在氢氧化钠水溶液中加热条件下,经开环水解制得丹曲林钠杂质B钠盐,再经盐酸酸化、精制合成了丹曲林钠杂质B,总收率16.9%,纯度99.9%,其结构经1H NMR,IR和MS(ESI)确证。
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| 关 键 词： | 丹曲林钠 开环 杂质 药物合成 |
Synthesis of Impurity B of Dantrolene Sodium |
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| ZHOU Yue-guang,TU Zeng-qing?,LUO Lan-qing,LI Guang-zhou,LI He. Synthesis of Impurity B of Dantrolene Sodium[J]. Chinese Journal of Synthetic Chemistry, 2017, 0(1). DOI: 10.15952/j.cnki.cjsc.1005-1511.2017.01.16189 |
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| Authors: | ZHOU Yue-guang TU Zeng-qing? LUO Lan-qing LI Guang-zhou LI He |
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| Abstract: | p-Nitrophenyl furfural ( 1 ) was synthesized by diazotization reaction of 5-nitroaniline with furfural. Dantrolene(2) was prepared by condensation of 1 with 1-aminohydantoin hydrochloride solu-tion, followed by refining. Dantrolene sodium(3) was prepared by reaction of 2 with sodium methox-ide. Impurity B of dantrolene sodium with the total yield of 16. 9% and purity of 99. 9% was obtained by hydrolysis of 3 in alkaline solution, then acidification with hydrochloric acid and recrystallization. The structure was confirmed by 1 H NMR, IR and MS( ESI) . |
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| Keywords: | dantrolene sodium ring opening impurity drug synthesis |
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