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1、河北工业大学硕士学位论文1，1，3，3-四甲基-2-环己基胍的合成及其在ADC合成反应中的应用姓名：孙潇磊申请学位级别：硕士专业：化学工艺指导教师：赵新强200803011,1,3,3-四甲基-2-环己基胍的合成及其在ADC合成反应中的应用PREPARATIONOFN-CYCLOHEXYL-N’,N’,N”,N”-TETRAMETHYLGUANIDINEANDITSAPPLICATIONINTHEREACTIONFORSYNTHESISOFADCABSTRACTGuanidineisanorganicstrongbaseandisusedasabasiccatalystorpro
2、moterinmanyreactions.Inthisthesis,N-cyclohexyl-N’,N’,N’’,N’’-tetramethylguanidine(CyTMG)wassynthesizedstartingfromtetramethylurea(TMU)andcyclohexylamineinthepresenceofphosphorusoxychloride(POCl3)catalystanditsstructurewascharacterized.ThenthereactionperformanceofCyTMGinthereactionforsynthesis
3、ofdiethyleneglycoldiallyldicarbonate(ADC)separatelybycarbondioxiderouteandtransesterificationroutewasevaluated.FinallyaseriesofN’,N’,N”,N”-tetramethyl-N–methyl-N-cyclohexylguanidiniumionicliquidsweresynthesized.ThepreparationconditionofCyTMGwasoptimizedbyorthogonaldesign.Underthefollowingcond
4、itions:n(TMU):n(POCl3)1:1，thereactiontimeaftertheadditionofphosphorusoxychloride11h，thereactiontimeaftertheadditionofcyclohexylamine36h,andthereactiontimeaftertheadditionofwater15minutes,theyieldofCyTMGwas50.1%.Andthestructureof1CyTMGwascharacterizedbymeansofIR,H-NMRandESI-MS.Inthecarbondioxi
5、deroutetoADCsynthesis,CyTMGnotonlyshowedagoodcatalyticactivitybutalsoservedasanacid-bindingagenttoabsorbHClproducedduringthereaction.BysodoingahugeamountofsolidwastegeneratedinthetraditionalroutewasavoidedandtheprocessforADCsynthesisbecamemuchcleaner.Thecatalystweightpercentage,reactioninitia
6、lpressure,moleratioofmaterials,reactiontemperatureandreactiontimewereoptimized.Underthefollowingconditions:reactiontemperature80℃,reactioninitialpressure4.0MPa,themolarratioofallylchloridetodiethyleneglycol6:1,themolarratioofdiethyleneglycoltoCyTMG3.4:1,andreactiontime12h,theyieldofADCattaine
7、d63.0%.AdditionallytherecoveryofCyTMGwas80.4%.InthetransesterificationroutetoADCsynthesis,CyTMGalsohadexcellentcatalyticactivity.Thereactionconditionswereoptimizedandtheproductdistributioninthereactionwasdiscussed.Undertheconditionsofthefirst
