| 柱前衍生化高效液相色谱法拆分1,1′-联-2-萘酚光学异构体 |
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| 引用本文： | 刘天穗,陈亿新,刘军涛,吴丹金,戴劲青. 柱前衍生化高效液相色谱法拆分1,1′-联-2-萘酚光学异构体[J]. 精细化工, 2007, 24(11): 1091-1094 |
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| 作者姓名： | 刘天穗 陈亿新 刘军涛 吴丹金 戴劲青 |
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| 作者单位： | 广州大学,化学化工学院,广东,广州,510006 |
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| 摘 要： | 以(S)-(+)-樟脑磺酰氯作柱前手性衍生化试剂,与外消旋1,1′-联-2-萘酚反应,形成非对映异构体联二萘酚樟脑磺酸酯,再用反相高效液相色谱进行分离。结果表明,采用Zorbax XDB-C8和HypersilODS(C18)柱,流动相V(甲醇)∶V(水)分别为75∶25和85∶15,流速均为1mL/min时,分离度分别为1.86和1.74,有效地分离了两个非对映异构体。进一步水解得到光学纯(R)-1,1′-联-2-萘酚和(S)-1,1′-联-2-萘酚,ee值均达99%以上。
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| 关 键 词： | 反相高效液相色谱 柱前衍生化 光学异构体拆分 1,1′-联-2-萘酚 (S)-(+)-樟脑磺酰氯 |
| 文章编号： | 1003-5214（2007）11-1091-04 |
| 修稿时间： | 2007-03-04 |
Separation of 1,1''''-Bi-2-naphthol Optical Isomers by High Performance Liquid Chromatography with Precolumn Derivatization |
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| LIU Tian-sui,CHEN Yi-xin,LIU Jun-tao,WU Dan-jin,DAI Jin-qing. Separation of 1,1''''-Bi-2-naphthol Optical Isomers by High Performance Liquid Chromatography with Precolumn Derivatization[J]. Fine Chemicals, 2007, 24(11): 1091-1094 |
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| Authors: | LIU Tian-sui CHEN Yi-xin LIU Jun-tao WU Dan-jin DAI Jin-qing |
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| Affiliation: | College of Chemistry and Chemical Engineering, Guangzhou University, Guangzhou 510006, Guangdong, China |
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| Abstract: | As the precolumn derivating agent,(S)-(+)-camphorsulfonyl chloride reacted with the racemic (±)-1,1′-bi-2-naphthol,producing two diastereomers of bis((S)-camphorsulfonates).Then the diastereomers were separated by reverse-phase high performance liquid chromatography.The result showed that the Zorbax XDB-C8 or Hypersil ODS(C18) column and V(methanol)∶V(water)=75∶25 or 85∶15 as eluent at a flowrate of 1 mL/min are suitable for the separation.Hydrolysis of the eluent gave optically pure (R)-and (S)-1,1′-bi-2-naphthol with ee > 99%. |
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| Keywords: | reverse-phase high performance liquid chromatography precolumn derivatization resolution of optical isomer 1,1′-bi-2-naphthol (S)-(+)-camphorsulfonyl chloride |
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