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L-苯丙氨酸手性固定相的制备 被引量:2

Preparation of L-Phenylalanine Chiral Stationary Phase
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摘要 L-苯丙氨酸和硬酯酰氯经酯化、酰胺化、皂化和酰氯化反应得到新型手性固定相,用FTIR、1HNMR和元素分析对手性固定相(CSP)进行了表征。将制得的手性固定相按m(CSP)∶m(硅胶)=3∶1制备薄层色谱板,采用V(乙醇)∶V(乙酸乙酯)∶V(三乙胺)=11∶5∶1作为展开体系,对手性药物度洛西汀进行拆分,其中右旋度洛西汀Rf1=0.87,左旋度洛西汀Rf2=0.75。 L-Phenylalanine CSP was prepared from L-phenylalanine and stearoyl chloride via esterifieation, amidation, saponification and acid chloride reaction. The CSP was characterized by means of FTIR, 1HNMR spectra and elemental analysis. Thin layer chromatography was prepared from the CSP and silica gel based on a mass ratio of 3 : 1. Using the development system of V(ethanol) : V ( ethyl acetate) : V(triethylamine) = 11:5:1, duloxetine was separated on the TLC, with (R) -duloxetine Rfl = 0.87, (S) -duloxetine Rf2 = 0.75.
出处 《精细化工》 EI CAS CSCD 北大核心 2012年第3期272-275,共4页 Fine Chemicals
基金 河北省科技计划项目(基础研究)(08965110D)~~
关键词 L-苯丙氨酸 衍生物 手性固定相 薄层色谱 手性拆分 分离提纯技术 L-phenylalanine derivatives chiral stationary phase thin layer chromatography chiralseparation separation and purification technology
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  • 1赵艳,姚金水,戴罡,呼建强.以氨基酸为手性源制备手性固定相的研究进展[J].山东轻工业学院学报(自然科学版),2008,22(4):1-3. 被引量:2
  • 2Barbara Wenzel,Steffen Fischer,Peter Brust,et al.Enantioseparation of vesamicol and novel vesamicol analogs byhigh-performance liquid chromatography on different chiralstationary phases[J].Journal of Chromatography A,2010,1217:3855-3862.
  • 3Giovanna Cancelliere,Alessia Ciogli,Ilaria D'Acquarica,et al.Transition from enantioselective high performance to ultra-highperformance liquid chromatography:a case study of a brush-typechiral stationary phase based on sub-5-micron to sub-2-micronsilica particles[J].Journal of Chromatography A,2010,1217:990-999.
  • 4Peng Liming,Jayapalan Swapna,Chankvetadze Bezhan,et al.Reversed-phase chiral HPLC and LC/MS analysis with tris(chloromethylphenylcarbamate)derivatives of cellulose andamylose as chiral stationary phases[J].Journal of ChromatographyA,2010,1217:6942-6955.
  • 5Michael Lmmerhofer.Chiral recognition by enantioselective liquidchromatography:mechanisms and modern chiral stationary phases[J].Journal of Chromatography A,2010,1217:814-856.
  • 6Kumar V Pavan,Reddy M Somi,Narender M,et al.Aqueous phasemono-protection of amines and amino acids as N-benzyloxycarbonylderivatives in the presence ofβ-cyclodextrin[J].TetrahedronLetters,2006,47:6393-6396.
  • 7Ali Thaqi,Adam McCluskey,Janet L Scott.A mild Bocdeprotection and the importance of a free carboxylate[J].Tetrahedron Letters,2008,49:6962-6964.
  • 8张庆合,张玉奎,李彤,等.一种粒径均一高纯硅胶微球高效液相色谱填料的制备方法[P].CN:00134301,2002-07-10.
  • 9何晓强.抗抑郁药盐酸度洛西汀的合成工艺改进[J].化学试剂,2010,32(3):266-268. 被引量:2
  • 10Zhou Ailing,Lu Xianyu,Xie Yunxuan,et al.Chromatographicevaluation of perphenylcarbamoylatedβ-cyclodextrin bondedstationary phase for micro-high performance liquidchromatography and pressurized capillary electrochromatography[J].Analytica Chimica Acta,2005,547:158-164.

二级参考文献24

  • 1贾湘曼.手性药物的研究与制备[J].承德医学院学报,2005,22(2):146-148. 被引量:2
  • 2Gerald Gubitz, Martin G. Schmid. Chiral separation principles in chromatographic and dectromigration techniques[J]. Molecular Biotechnology, 2006, (32) : 159 - 179.
  • 3殷元骥,蒋耀忠.不对称催化反应进展[M].北京:科学出版社,2000.
  • 4L. Vaton chanvrier, Y. Combret, J.C. Co - mbret. High - performance liquid chromatographic investigation of the enantioselectivity and mechanism of chiral recognition of new cholic acid - based stationary phases[J]. Chromatographia, 2001,54(7) :31 - 37.
  • 5STASZAK M A, WELGEL L O.'Chiral synthesis of 1-aryl-3- aminopropan- 1- ols: EP, 0 457 559 [ P ]. 1991-11-21.
  • 6DEETER J,FRAZIER J, STATEN G, et al. Asymmetric synthesis and absolute stereochemistry of LY248 686[J]. Tetrahedron Leu. , 1990,31(49) :7 101-7 104.
  • 7BERGLUND R A.Asymmetric synthesis:US,5 362 886[ P]. 1994-11-08.
  • 8WHEELER W J, KUO F J. An asymmetric synthesis of duloxetine hydrochloride, a mixed uptake inhibitor of serotonin and norepinephrine,and its C-14 labeled isotopomers. [J].Label Compd . Radiopharm . , 1995,36(3) :213-223.
  • 9LIU Hui-ling, HOFF B H, ANTHONSEN T. Chemo-enzymatic synthesis of the antidepressant duloxetine and its enantiomer [ J ]. Chirality, 2000,12( 1 ) : 26-29.
  • 10ROBERTSON D W, WONG D T, KRUSHINKI Jr, et al. 3- Aryloxy-3-substituted propanamines : US, 5 023 269 [ P ]. 1991-06-11.

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