两种酰胺型手性物的合成和拆分性能测定以与新型手性试剂光学纯度测定方法.研究

两种酰胺型手性物的合成和拆分性能测定以与新型手性试剂光学纯度测定方法.研究

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时间:2019-01-30

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1、四川大学硕士研究生毕业论文selectorsweredetectedbyPhoto—Diode-ArraydetectorandOptical.Rotationdetectorofhi曲performanceliquidchromatography.Themethodseparatedtheracemateisestablished,andthisisusefulforfurtherstudyofchiralseparationmechanism.㈣-2-thiothiazolidine-4-carboxylicacidisoneofthechiralresolutivereag

2、ents,andCallseparatetheracemates,such嬲aminoacylesters,aminoalcohol,andphenylethylamineandSOon.Thedirectseparationoftheracernate.2-thiothiazolidine一4-carboxyticacid,byhighperformanceliquidchromatographyisunrecorded.Astheusefulchiralseparationreagents,itisunfeaSiblethatthespecialrotationisjustn

3、oted,buttheenantiomericpurityisnotreported.ThisCaninfluenceonitssyntheticoptimization,andpreventitsapplications.Inthisthesis,thedirectseparationconditionsoftheracemateof2-thiothiazolidine一4一carboxylicacidonDNB—LencinecsP,DNB—PGCSP,Whelk—01CSPandOD—HCSPwerestudied,butfailed.The2-thiothiazolidi

4、ne--4--carboxylicacidWaSderivatizedwithanilinewhichwasthereagentofpre·columnderivatizationofhighperformanceliquidchromatography.ThederivativewasseparatedbyDNB—Lencinechiralstationaryphase,anddetectedbyPhoto-Diode-ArraydetectorandOptical·-Rotationdetector.Themethodwhichseparatedtheracemateandd

5、eterminedtheenantiomericpurityof2-thiothiazolidine·4·carboxylicacidWasestablished.ChromatographicmodelWasemployedforenantionmericseparationof2-thiothiazolidine-4一carboxylicacidderivativesontheDNB—LeucinechiralCOlumninhexane/alcohol(ethanolorisopropylalcoh01)mobilephase.Theeffectsofchromatogra

6、phyconditions,such嬲mobilephasesandtemperaturetochiralrecognition,hadbeeninvestigated.Abetterconditionofanalysiswasobtained,andtheseparationfactorWaSmorethan1.2.Furthermore,theresultsofenantiomericpuritydeterminedbypolarimeterandHPLCwereveryconsistent,andtherelativedeviationWaSnotmorethan1.34%

7、.Themethodofpre—columnderivatizationofhighperformanceliquidchromatographyiscredible,accurateandCanbeappliedtodetermineenantiomericpurityof2-thiothiazolidine-4-carboxylicacid.Theeffectsofconcentrationandtemperatureonspecialrotationof(R)-2·thio

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