| (S)-(+)3-氨基吡咯烷二盐酸盐的合成研究 |
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| 引用本文： | 蒋旭东,袁哲东.(S)-(+)3-氨基吡咯烷二盐酸盐的合成研究[J].精细石油化工,2013,30(3):35-38. |
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| 作者姓名： | 蒋旭东 袁哲东 |
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| 作者单位： | 1. 广西工学院生物与化学工程学院,广西柳州545006;上海医药工业研究院创新药物与制药工艺国家重点实验室,上海200437
2. 上海医药工业研究院创新药物与制药工艺国家重点实验室,上海,200437 |
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| 基金项目： | "国家重大新药创制"科技重大专项资助，上海市优秀学科带头人计划项目 |
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| 摘 要： | 以L-天冬氨酸为原料,经缩合得N-甲酰-L-天冬氨酸酐,然后经酰化、酯化、还原、成环得(S)-1-苄基-3-氨基吡咯烷,最后脱苄合成(S)-(+)3-氨基吡咯烷二盐酸盐,总收率62.8%。考察了工艺条件对反应的影响。(S)-1-苄基-3-氨基吡咯烷适宜工艺条件为:n(KBH4)∶n(H2SO4)∶n(混合物4)=3∶1.5∶1,反应温度50～60℃,反应时间6h,收率71.6%。产物结构经MS和1 H NMR进行确证。
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| 关 键 词： | L-天冬氨酸 (S)-(+)-3-氨基吡咯烷二盐酸盐 合成 |
SYNTHESIS OF (S)-(+)-3-AMINOPYRROLIDINE DIHYDROCHLORIDE |
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| Jiang Xudong
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Yuan Zhedong.SYNTHESIS OF (S)-(+)-3-AMINOPYRROLIDINE DIHYDROCHLORIDE[J].Speciality Petrochemicals,2013,30(3):35-38. |
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| Authors: | Jiang Xudong Yuan Zhedong |
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| Affiliation: | 1.Department of Biological and Chemical Engineering,Guangxi University of Technology,Liuzhou545006,Guangxi,China;2.State Key Lab of New Drug and Pharmaceutical Process,Shanghai Institute of Pharmaceutical Industry,Shanghai 200437,China) |
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| Abstract: | N-Formyl-L-aspartic anhydride was prepared via condensation reaction with L-aspartic acid,then the compound(S)-1-benzylpyrrolidin-3-amine was obtained from N-formyl-L-aspartic anhydride via acylation,esterification,reduction and ring closing,finally(S)(+)-3-Aminopyrrolidine dihydrochloride was obtained through debenzylation with the total yield of 62.8%.The effect of synthesis conditions on(S)-1-benzylpyrrolidin-3-amine was studied.The optimal reaction conditions were found as follows : the yield could reach 71.6% when n(KBH 4) ∶n(H 2 SO 4) ∶n(Compound 4) =3∶1.5∶1 and reacted 6hat 50-60℃.The target compound was confirmed by MS and 1 H NMR. |
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| Keywords: | L-aspartic acid (S)(+)-3-aminopyrrolidine dihydrochloride synthesis |
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