| 甲磺酸达比加群酯杂质的合成 |
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| 引用本文： | 高航,宗新杰,陈会慧,刘长鹰,王松会,李川,徐为人.甲磺酸达比加群酯杂质的合成[J].合成化学,2015,23(11):1068-1073. |
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| 作者姓名： | 高航 宗新杰 陈会慧 刘长鹰 王松会 李川 徐为人 |
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| 作者单位： | 1. 天津医科大学 研究生院，天津 300070； 2. 天津中医药大学 研究生院，天津 300193; 3. 天津药物研究院有限公司 天津市新药设计与发现重点实验室，天津 300193 |
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| 摘 要： | 根据甲磺酸达比加群酯工艺，合成了甲磺酸达比加群酯的7个杂质：3-【【【2-｛［(4-氰基苯基)氨基］甲基｝-1-甲基-1H-苯并咪唑-5-基】羰基】(吡啶-2-基)氨基】丙酸（A）, 3-【【【2-【｛［4-(乙氧基)叔胺基］苯基｝氨基】甲基】-1-甲基-1H-苯并咪唑-5-基】羰基】(吡啶-2-基)氨基】丙酸乙酯盐酸盐(B), 3-【【【2-【｛［(4-甲脒基)苯基］氨基｝甲基】-1-甲基-1H-苯并咪唑-5-基】羰基】(吡啶-2-基)氨基】丙酸乙酯盐酸盐(C), 3-【【【2-【【【4-｛［(己氧基)羰基］氨基亚甲胺基｝苯基】氨基】甲基】-1-甲基-1H-苯并咪唑-5-基】羰基】(吡啶-2-基)氨基】丙酸甲酯盐酸盐(D), 3-【【【2-【【【4-【｛［(己氧基)羰基］氨基｝羰基】苯基】氨基】甲基】-1-甲基-1H-苯并咪唑-5-基】羰基】(吡啶-2-基)氨基】丙酸乙酯(E), 3-【【【2-【【【4-【｛［(己氧基)羰基］氨基｝亚氨甲基】苯基】氨基】甲基】-1-甲基-1H-苯并咪唑-5-基】羰基】(吡啶-2-基)氨基】丙酸(F), (Z)-3-【【【2-【【【4-【｛［(N,N′-二己氧基)羰基］脒基｝亚氨甲基】苯基】氨基】甲基】-1-甲基-1H-苯并咪唑-5-基】羰基】(吡啶-2-基)氨基】丙酸乙酯(G)，其结构经1H NMR和ESI-MS确证。
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| 收稿时间： | 2015-06-24 |
Synthesis of the Impurities of Dabigatran Etexilate Mesylate |
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| GAO Hang,ZONG Xin-jie,CHEN Hui-hui,LIU Chang-ying,WANG Song-hui,LI Chuan,XU Wei-ren.Synthesis of the Impurities of Dabigatran Etexilate Mesylate[J].Chinese Journal of Synthetic Chemistry,2015,23(11):1068-1073. |
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| Authors: | GAO Hang ZONG Xin-jie CHEN Hui-hui LIU Chang-ying WANG Song-hui LI Chuan XU Wei-ren |
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| Institution: | 1. Graduate school, Tianjin Medical University, Tianjin 300070, China; 2. Graduate school, Tianjin University of Chinese Traditional Medicine, Tianjin 300193, China; 3. Tianjin Key Laboratory of Molecular Design and Drug Discovery， Tianjin Institute of Pharmaceutical Research Co., Ltd, Tianjin 300193, China |
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| Abstract: | According to the synthetic route of dabigatran exetilate mesylate, seven kinds of impurities were synthesized: 3-【【【2-｛［(4-cyanophenyl)amino］methyl｝-1-methyl-1H-benzimidazol-5-yl】carbonyl】pyridin-2-ylamino】propionic acid(A), ethyl 3-【【【2-【｛［4-(ethoxy) tertiary amine］phenyl｝amino】methyl】-1-methyl-1H-benzimidazol-5-yl］carbonyl】pyridin-2-ylamino】propanoate hydrochlorid(B), ethyl 3-【【【2-【｛［(4-N′-methylcarbamimidoyl)phenyl］amino｝methyl】-1-methyl-1H-benzimidazol-5-yl】carbonyl】pyridin-2-ylamino】propanoate hydrochlorid(C), methyl 3-【【【2-【【【4-｛［(hexyloxy)carbonyl］carbamimidoyl｝phenyl】amino】methyl】-1-methyl-1H-benzimidazol-5-yl】carbonyl】(pyridin-2-yl)amino】propanoate hydrochlorid(D), ethyl 3-【【【2-【【【4-【｛［(hexyloxy)carbonyl］amino｝carbonyl】phenyl】amino】methyl】-1-methyl-1H-benzimidazol-5-yl】carbonyl】(pyridin-2-yl)amino】propanoate(E), 3-【【【2-【【【4-｛［(hexyloxy)carbonyl］carbamimidoyl｝phenyl】amino】methyl】-1-methyl-1H-benzimidazol-5-yl】-carbonyl】(pyridin-2-yl)amino】propanoic acid(F), ethyl (Z)-3-【【【2-【【【4-{［(N,N′-bishexyloxy)carbonyl］carbamimidoyl｝phenyl】amino】methyl】-1-methyl-1H-benzimidazol-5-yl】carbonyl】(pyridin-2-yl)amino】propanoate(G). The structures were confirmed by 1H NMR and ESI-MS. |
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