紫罗兰酮的合成研究

©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.:(1952-),,.:1006-0456(2006)03-0223-04,,,(,330029):,,,,..:0.18mol,n()zn()zn()=1z6z1.5,(NaOH)1.5%,5060,77.75%.NaOH/,3%5%,12h.:15g,62%H2SO430g,18.45g,2030,68.33%.:;;;;;:O621.3:A,.--,.:,[1].[1-2],,[3].,2%4%,75%,,55.9%,,.,,[4].,-,.-MCF-7DNA,,.,-A.,,.,,,,.,[5].,,,[6].,.11.11.1.12W.1.1.298%,(CP),NaOH(CP),(CP),(CP),(CP),(CP),,,.1.228320069JournalofNanchangUniversity(Engineering&Technology)Vol.28No.3Sept.2006©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.():m(98%)zm(95%)zm(1.5%NaOH)=1z2z2.:34.693g80g80g1.5%NaOH502h,603h,30min,,10%(),,,,,,124144/799.932Pa.1.3.2():m()zm(62%H2SO4zm()=1z1.5z1.23.:22.5g62%H2SO4,18.45g,2015g,20.30min,36,30min,10g,,,,25mL,10%(pH89),10%(pH56).,120124/1.333kPa.22.128g80g1.5%NaOH,,,502h,603h,,30min,,10%(),,,,,.1.1Fig.1Effectofacetonecontentonyield,60g,.60g,..2.260g80g1.5%NaOH,,,2.1,2.2Fig.2Effectofcitralcontentonyield4222006©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.:,28g,60g80g1.5%NaOH,,1:,.,.,,.2.422.5g62%H2SO415g,,,20,30min,36,,3.3,18.45g,.18.45g,.25.9540.95g,,..2.5H2SO418.45g15g,,62%H2SO4,20,30min,36,,4.3Fig.3Effectofbenzenecontentonyield4H2SO4Fig.4Effectofcatalystsulfuricacidcontentonyield4H2SO4.62%H2SO430g,45g,,.--,,-.,62%,,.2.622.5g62%H2SO4,15g,18.45g,,30min,36,,5.5,.10,5223:©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.:5060,2.53h,,,.n()zn()1z6,,77.75%.,,.,,,.,,.15g62%H2SO430g18.45g,2030,68.33%.:[1].[J].,1998,15(4):60-62.[2].[J].,1959(7):338-339.[3].[J].,1955(9):439-442.[4].[J].,1998,25(1):54-56.[5].[J].,1993(3):21-25.[6],.-[J].,2002,19(3):132-136.StudyonSynthesisofIononeWUQin2fen,LIUYan2yan,ZHUZhi2wu,WANGYu(SchoolofEnvironmentalScienceandEngineering,NanchangUniversity,Nanchang,330029,China)Abstract:Thesynthesisofiononefromnaturalcitralthroughtwo-stepreactionsofcondensationandcycliza2tionwasinvestigated.Theeffectsofcatalystsandsolvents,alsotheratioofreagentsandtemperatureonreactionwerediscussed.Theresultsshowedthattherateofcondensationachieved77.5%atn(citral)zn(acetone)zn(majorcatalyst)=1z6z1.5,concentrationofmajorcatalyst(NaOHsolution)5%,reactiontemperature5060.ThetotalyieldofIononeaftercyclizationwas68.33%obtainedoncondition:pseudo-ionone15g,62%sul2furicacid30g,benzene18.45g,reactiontemperature2030.Theyieldofcondensationwasfoundimprovedby3%5%bytheuseofphasetransfercatalyst(NaOHsolution),andthereactionperiodwasshortened.KeyWords:citral;acetone;condensation;cyclization;pseudo-ionone;ionone6222006