简介:THEREACTIONOFp-NITROPHENYLSULFONYLACETONITRILEWITHα,β-UNSATURATEDESTERSANDNITRILES¥GuoRenYUEandZhengZhang(DepartmentofChemist...
简介:InanefforttoutilizeNMRtechniquefortheanalysisofthestructuralcomponentsofwoodandbiomassessuchaslignin,wemadeacomparativestudyoflignincontentsofseveraltypesoflignocellulosicmaterialsbothbeforeandafterenzymatichydrolyses.Tothisend,EucalyptusGlobulus,Norwaysprucethermomechanicalpulp(TMP)cornstoverandEucalyptuskraftpulpwereball-milledandtreatedwithcellulasetopreparematerialswithhighlignincontents.Thesematerialswereanalyzedvia31PNMRinionicliquids.Theresultsshowthatthecontentsofvariousfunctionalgroupsforthelignocellulosicmaterialsafterenzymatichydrolysesaregenerallyinagreementwiththosefromtheircorrespondingenzymaticmildacidolysisliginins(EMALs),indicatingthat31PNMRanalysisoflignocellulosicmaterialsinionicliquidsisapromisingmethodforquantitativecharacterizationoflignocellulosicmaterials.
简介:π-Conjugatedpoly(p-phenyleneethynylene)withtheinterruptionoftheconjugationbyabutyleneunitwassynthesized.Itsabsorption,PLandELspectrawereinvestigatedrespectively.Thespectralpeaksshiftedtothehigherenergysidewiththeinterruptionoftheconjugationlengths.Themodelcompoundwassynthesized,bywhichtheresultswereproved.ThethermalcharacteristicsofthepolymerwasdeterminedbyDSCandTGA,indicatingthatthepolymerhasagoodthermalstability.Theelectroluminescence(EL)inthegreenregionofthespectrumwithamaximumat500nmwasobservedfromthepolymerfilmssandwichedbetweenindium-tin-oxideandanAlelectrode.
简介:AnovelacrylicmonomerbearingaromaticetherealitygroupN-(p-phenoxy-phenyl)methacrylamide(MAPOA)wassynthesizedandpolymerized.ThefluorescencespectraofMAPOAanditspolymerwerestudied,showingthatthepolymerdisplaysastrongerfluorescencethanitsmonomeratthesamechromophoreconcentration.ThefluorescenceofP(MAPOA)wasquenchedbyaddingelectrondeficiencymonomerssuchasMMA,ANetc..Itisanotherexampleofshowingthe"fluorescencestructuralself-quenchingeffect"aswereportedpreviously,fromwhichitisdemonstratedagainthatthisphenomenonisnotanaccidentalonebutacommoneffectforacrylicmonomersbearingelecton-donatingchromophores.ThephotopolymerizationofANsensitizedbyMAPOAandP(MAPOA)wasstudied.Thekineticequationofthepolymerizationwasobtainedandrepresentedasfollows:Rp∝[MAPOA]0.38×[AN]0.78,Rp∝[P(MAPOA)]0.33×[AN]0.71TheoverallactivationenergiesweredeterminedtobeEa=24.22kJ/mol(MAPOA)andEa=26.31kJ/mol[P(MAPOA)]respectively.ThefluorescenceanalysisoftheresultedP(AN)showedthatthesensitizeralsoenteredintotheP(AN)chains.AmechanismoftheformationofachargetransfercomplexandfreeradicalinitiationwassuggestedforthephotopolymerizationofANsensitizedbyMAPOAandP(MAPOA).
简介:Apartiallysubstitutedβ-cyclodextrinchiralstationaryphasewaspreparedbythereactionofphenylisocyanate.TheenantiomersofaseriesofO,O-diethyl(p-methylbenzenesulfonamido)-aryl(oralkyl)-methylphos-.phonateswerestudiedonthepreparedphenylcarbamatederivativeβ-cyclodextrinbondedphaseandacommercial(S)-(.+)-l-(l-naphthyl)ethylcarbamatederivativeβ-cyclodextrinbondedphaseonnormalphasechromato-graphiccondition.Resultsshowthatthepreparedphenylcarbamatederivativeβ-cyclodextrinbondedphasehasbetterenantiomericselectivitytotheseriesofcompounds.Achiralrecognitionmechanismwassuggestedfortheseparationofthesenovelorganicphosphorusenantiomers.
简介:IntroductionThesynthesesandcharacterizationofporphyrinsandmetalloporphyrinshavebeenstudiedextensively[1].Hemoglobin,myoglobinorcytochromeP450,hasbeenappliedasamodelcompound[2].WongC.P.etal.[3]synthesizedthefirstlanthanideporphyrin,acetylacetonatetetraphenylporphyrineuropium,in1974.
简介:Thetitlecopolymer(PDEBO)wassynthesized.ThethermalcharacteristicsofthepolymerweredeterminedbymeansofDSCandTGA,revealingthatthepolymerhasagoodthermalstability.TheX-raydiffractionmeasurementsofthethinfilmsshowedthatthepolymerisdisorder.Electroluminescence(EL)inthegreenregionofthespectrumwithamaximumat500nmwasobservedfromthepolymerfilmssandwichedbetweenindium-tin-oxideandanAlelectrode.
简介:为了探索二氢杨梅素半合成杨梅素作用机理,依据文献中提出的最佳反应条件,并进行重复验证,同时利用高效液相色谱对反应过程进行痕迹跟踪.实验结果表明:二氢杨梅素在最佳反应条件下搅拌反应,杨梅素的生成率为11.2%,与文献值基本符合.然而,液相色谱并没检测到文献中提出的查尔酮结构中间体和环氧烷结构中间体.另外,分别探讨了氢氧化钠用量与生成查尔酮结构中间体和杨梅素生成率之间的关系.实验结果表明:二氢杨梅素在1%的氢氧化钠水溶液(5.5mL)、恒温水浴35℃搅拌20h,反应过程通过液相色谱跟踪,并未检测到对应的查尔酮结构中间体生成,却检测到杨梅素成分的生成痕迹;随着反应时间的延长,杨梅素生成率逐渐升高,可达65.1%.最后,利用电子顺磁共振波谱仪(EPR)对二氢杨梅素在碱性环境中释放超氧阴离子的行为进行观察.结果表明:二氢杨梅素溶于弱碱性(pH值为8~9)的甲醇(φ=50%)溶液中,且有氧条件下,加入自旋电子捕获剂DMPO(5,5-二甲基-1-吡咯啉-N-氧化物)后,可观察到DMPO捕捉超氧阴离子形成的加合物特征峰,且随着时间的延长,其特征峰的强度也增强.综上所述,实验证实了文献中提出的二氢杨梅素半合成杨梅素作用机理的不合理性,并合理地提出了基于超氧阴离子催化二氢杨梅素脱氢合成杨梅素的作用机理.
简介:Aseriesofcarboxylate-substitutedtrinudearmolybdenumdus-tercompoundsformulatedasMo3S4(DTP)3(RCO2)(L),whereRffiH,CH3,C2H5,CH2Cl,CCl3,R^1C6H4(R^1isthegrouponthebenzeneringofaromaticcarboxylate),L=pyridine,CH3CN,DMF,havebeensynthesizedbytheligandsubstitu-tionreaction.Thedissociationoftheloosely-coordinatedligandLfromtheclustercorewasstudiedby^31pNMR.Thedissocia-tionprocessofLisrelatedtothesolvent,temperature,andacidityofcarboxylategroups,soastoaffectthesolutionstruc-tureandreactivepropertiesoftheduster.Thelong-distancein-teractionbetweenligandsRCO2andListransportedbyMo3S4core.
简介:ThermotropicliquidcrystallineVHEterpolyestersmadefromvanillicacid(V),p-hydroxybenzoicacid(H)andpoly(ethyleneterephthalate)(E)werestudiedby400MHzNMRspectra,wideangleX-raydiffraction,scanningelectronandpolarizingmicroscopes.ItwasfoundthattheVHEterpolyestershadrandomsequencedistribution.TheVHEterpolyesterfilmsexhibitedhighlyorientedfibrillarstructure.
简介:Thecompleteaminoacidsequenceofβ-momorcharin,aribosome-inactivatingproteinfromtheseedsofMomordicacharantiaLinn(Cucurbitaceae)hasbeendetermined.Thishasbeendonebythesequenceanalysisofpeptidesobtainedbyenzymaticdigestionwithtrypsin,chymotrypsinandS.aureusV8protease,aswellasbychemicalcleavagewithBNPS-skatole.Theproteinconsistsof249aminoacidresiduescontainingoneasparagine-linkedsugargroupattachedtothesiteofAsn51andhasacalculatedrelativemolecularmassof28,452Dawithoutadditionofthecarbohydrate.Comparisonofthissequencewiththoseoftrichosanthinandotherribosome-inactivatingproteinsfromdifferentspeciesofplantsshowsasignificanthomologywitheachother.Regardingthesimilarityoftheirbiologicalproperties,anactivedomainoftheseproteinshasbeenpredictedhere.
简介:Fivechiralstationaryphases(CSPs)wereusedtoseparatetheenantiomersofaseriesofO,O-diethyl(p-methyl-benzenesulfonamindo)-aryl(alkyl)-methylphosphonates.Achiralrecognitionmechanismwaspresentedtoexplaintheresolutionofthesecompounds.ResultsshowthatCSPwithstrongπ-acceptor3,5-dinitrobenzoylgroupandhighsterichindrancehasthebestresolutionabilityinchiralseparationofO,O-diethyi(p-methyl-benzenesulfonamindo)-aryl(alkyl)-methylphosphonates.WhenaCSPhasjustastrongπ-acceptor3,5-dinitrobenzoylorhighsterichindranceitdoesnothavegoodchiralresolutionability.ThechiralrecognitionismoredifficultwhentheCSPhasmorethanoneasymmetriccenter.
简介:Theseparationofenantiomersofaseriesofeighteennovelnitrogenmustardlinkedphosphoryldiamidederivativeswasinvestigatedonthepreparedphenylcarbamatederivativeβ-cy-clodextrinbondedphaseinnormal-phaseHPLC.Someoftheenantiomerscouldbeseparatedinbaseline.Thechiralrecognitionmechanismwasalsosuggestedfortheseparationofchiralphosphorusorganiccompounds.
简介:目前,国内没有关于半钢发热剂的国家标准检测方法,只能根据组分范围分别检测各个组分,不仅耗时而且使用的大量化学试剂对环境造成污染。故研究了X-射线荧光光谱法快速测定半钢发热剂中Si,P,S的方法。采用粉末压片制样,研究其制样条件,包括磨样时间、压样时间和压力对测定结果的影响。采用其它方法定值提供的检测样品,作为x-射线荧光光谱法内控标准样品,采用经验系数法进行基体校正,通过解谱拟合建立校准曲线,校准曲线建立后仪器建立漂移校正程序。实验结果精密度好,各元素的相对标准偏差在0.15%-1.3%。准确度满足生产需求,实验方法可用于快速检测半钢发热剂化学组分。