spectroscopical investigation of some …：一些光谱研究…

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1、SPECTROSCOPICALINVESTIGATIONOFSOMECALIX[N]ARENESDERIVATIVES…SPECTROSCOPICALINVESTIGATIONOFSOMECALIX[N]ARENESDERIVATIVESUTILISABLEASMETALEXTRACTINGAGENTSCRISTINACIOCAN,ELISABETH-JEANNEPOPOVICI,CRINADAN,MARIAVĂDAN,RODICAGRECUandN.POPOVICI“RalucaRipan”InstituteofChemistry,30Fântânele,3400-Cluj-NapocaR

2、OMANIAABSTRACT.p-tert-butil-calix[n]arene[n=4,6]andtheircorrespondingacetate-derivativeswerepreparedbyspecificprocedures.Thecalix[n]arenes'puritywascheckedbyelementalanalysisandvariousspectroscopicmethodssuchasRMN,MS-GC,UV-VisandFTIR.Theabilityofcalixarenesacetatestoextractpreciousmetallicionsfroma

3、queoussolutionswastested.ThehigheffectivenessofO-acetilatedp-t-butilcalix[6]arenetoextractPt(II)ionswasdemonstratedinrelationwithPd2+andRh3+species.Keywords:calixarenes;liquidextraction;preciousmetalionsextraction.1.INTRODUCTIONCalix[n]arenesarepolinuclearcompoundsthatactasselectivecomplexationagen

4、tsforelectricalchargedorneutralspecies.Thehighcomplex-formationabilityofcalix[n]arenesoffersthemlargeutilizationpossibilitiesinthemanufactureofsensitivemembranes,elaborationofsomeselectiveextractionmethodsforvariouscationsandanions,realizationofmodernmetalrecoveryproceduresandfortheenvironmentalpro

5、tection.ThepurposeofthisstudyistopresentourattempttopreparesomeO-acetilatedp-tert-butil-calix[n]areneinordertotesttheirabilitytoco-ordinatepreciousmetallicions.2.EXPERIMENTALPARTp-tert-butyl-calix[4]areneandcalix[6]arenewerepreparedandpurifiedbyC.D.Gutsche'technique1,2.Theasmentionedcalixareneswere

6、convertedintothecorrespondingacetatederivativesbyusingaceticacidanhydrideasO-acetilatingreagent(reaction#1).Inthisrespect,about2mmolofp-tert-butylcalix[n]arenewastreatedwith50mlofaceticacidanhydrideandtwodropsofconcentratedsulfuricacid3.Themixturewasheatedandrefluxedfor2hours.(1)Thecrudeproductwasr

7、ecrystallisedfromchloroform/methanol.Whiteplateletswereobtainedwithayieldof45-47%.ThepurityofaspreparedproductswascheckedoutbyelementalanalysisaswellasbyIR,UV-Vis,1HNMRandmassspectroscopy.455SPECTROSCOPICAL