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乙酸肉桂酯的合成乙酸肉桂酯的合成ContentsIntroduction1Experimental2Results&discussion34ConclusionsL-LPTCItinvolvesthe
reactionofanionicreactant
fromaqueousphasewiththereactantinorganicphasebyaphasetransfercatalystS-LTPCItinvolves
thereactionbetweenthesolidnucleophilewiththeotherreactant
intheorganicliquidphasePTCphasetransfercatalysisItinvolvesthereactionofanionicreactantfromaqueousphasewiththereactantinorganicphasebyaphaseaddarequiredsurfaceareaandmasstransferlimitations.Results&discussionExperimentalreactiontemperaturephasebyaphaserateexpressionrateexpressioninthefollowingstudies.‘‘omegaphase”enhancetheItinvolvesthereactionofanionicreactantfromaqueousphasewiththereactantinorganicraisedto90°CwithExperimentalreached90°CL-LPTC
eliminatesthe
needofusingaqueousphasethuseliminatestheseparationproblems
andeasyrecoveryofthecatalystenhancestheproductselectivitybyavoidingthesidereactionslowerselectivityandothersidereactionssynthesis
offineandspecialtychemicalsseparationand
purifyingthefinalproductComparedwithL-LPTCandL-SPTCL-SPTCthecarboxylicacidsshowslessreactivity‘‘omegaphase”enhancethesolubilizationofthesolidandformationofthecatalyticintermediatewefocusoureffortsonstudyingthekineticsandfactorsaffectingthesynthesisofcinnamylacetate(乙酸肉桂酯)fromcinnamylbromide(肉桂酸溴)andsodiumacetate(乙酸钠)byS–LPTC.
sodiumacetate(0.025mol),cinnamylbromide(0.02mol),n-dodecaneadd
chlorobenzeneto
50mLandthetemperature
was
raisedto90°CwithconstantstirringProductaddarequiredamountofphasetransfercatalystwhenthe
temperaturereached90°C
Atpresettimes,thestirrer
wasturne
offtemporarily,0.5mloforganicsolutionwas
pipettedoutanalyzedonagaschromatographusingSE-30Column.3.Results&discussion7factorstypeofcatalystspeedofagitationreactiontemperaturewateradditionsizeofsodiumacetatecatalystloadingconcentrationofreactantInordertooptimizethereactionconditions,theesterificationreactionwascarriedoutbyvaryingfactorsasfollow:
3.Results&discussion3.1EffectofagitationspeedTheinterfacialmasstransferresistancebetweenthesolidsurfaceandorganicphaseisnegligiblewhentheagitationspeedisabove600rpm.Inthiscontext,agitationspeedwasfixedat600rpmforallfurtherexperiments.
3.Results&discussion3.2EffectofalkylchainlengthofthecatalystHenceTBABischosenasthephasetransfercatalystinthefollowingstudies.3.Results&discussion3.3effectofreactiontemperatureAlthoughahightemperatureusuallyfavorsthesidereactions,nosideproductswerefoundat95°Cinthisstudy.3.Results&discussion3.4EffectofcatalystloadingSincereasonableconversionsareobservedatthecatalystloadingof1.6g,thefurtherexperimentsarecarriedoutatthecatalystloadingof1.6g.ItinvolvesthereactionofanionicreactantfromaqueousphasewiththereactantinorganicTheinterfacialmasstransferresistancebetweenthesolidsurfaceandorganicrateexpression5andremainedalmostconstantthereafter.Inthiscontext,agitationspeedwasfixedat600rpmforallfurtherexperiments.solubilizationofthesolidandformationofthecatalyticintermediatephasetransfer6、Thereactionresultsobtainedat80–95Cwellfittedintothepseudo-firstorderrateequation.phaseisnegligiblewhentheagitationspeedisabove600rpm.Results&discussion2、Usingamoderateamount(1.Results&discussiontypeofcatalyst6g)oftetran-butylammoniumbromideasthecatalystat95°C.
3.Results&discussion3.5EffectofmoleratioTheconversionofcinnamylbromideincreasedwiththeincreaseofmoleratioofcinnamylbromidetosodiumacetatefrom1:1to1:1.5andremainedalmostconstantthereafter.
3.Results&discussion3.6EffectofwateradditionTheoptimalusageofwaterinthepresentstudywasobservedtobe4ml.
3.Results&discussion3.7EffectofpaticalsizeofsodiumacetateLowreactivityofthesodiumacetategranulesmaybeattributedtotheirlowsurfaceareaandmasstransferlimitations.3.Results&discussionrateexpression——(1)3.Results&discussionrateexpression——(2)3.Results&discussionrateexpressionk=k'Cc——(3)1、Thesolid–liquidphasetransfercatalysiswassuccessfullyemployedforthesynthesisofcinnamylacetatefromtheesterificationofsodiumacetatewithcinnamylbromidebyusingTBABasthecatalyst.2、Usingamoderateamount(1.6g)oftetran-butylammoniumbromideasthecatalystat95°C.3、Thesolid–liquidinterfacialmasstransferresistanceisnegligibleatagitationspeedabove600rpm.4、Thecatalystwithlongeralkylchainlengthgivesbetterperformance,however,itwillmoreeasilydissolvedintheorganicphaseandhenceismoredifficulttoberemovedandreusedafterthereaction.5、Adding1–8mlofwaterimprove
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