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1、SimpleandVersatileVacuumandPressureReactorsforAir-SensitiveMaterialsNeilBurford,JurgenMullerandTrentonM.ParksDalhousieUniversity,Halifax,NovaScotia,CanadaB3H4J3Withtheavailabilityofhighqualityinertatmosphereapparatus(dryboxes),efficientvacuumpumpsandelabo-ratevacuumsvstems.aswellasestabli
2、shedtechniauesforperformingalmostanyexperimentalmanipulationunderanatmosphereofdrynitrogen(Schlcnktechniques),thehandlingol'air-sensitivecompoundsposeslittleproblemtothemodernsyntheticchemist.However,manyofthepro-ceduresrequiredtomaintainpristineatmospheresinvolveeitherintricatemaneuversw
3、ithsophisticatedapparatusesorareincompleteintermsofrigorousexclusionofmois-tureorotherimpurities,suchasgrease.Moreover,theavailabletechniquestendtodevelovcharacteristicsoftheexperimentalistperformingtheoperationsandmayhavedeficienc~esthatarenotreadilyapparentorart:difficulttoreproduce.Asa
4、consequence,iti6raretofindanunder--maduateteachine-laboratowthatinvolvesthehundline-ofcriticallyair-sensitivematerials,despitethepredomi-nanceofsuchsubstancesinthecurrentliterature.Ourworkwithhighlyelectrophilicnonmetalcations(I)hasne-cessitatedthedevelo~mentofsim~le.versatile.robustandat
5、mosphericallyreliibleapparat;s,thatwefek~offersub-stantialbenefitsoverother,previouslyreportedsystems.Herewedescribethereactorsandtheproceduresthatal-lowustoperformsyntheticchemistryandanalysisunderanhydrousandanaerobicconditionswithrelativeease,andwithreproducibilityandsimplicityappropri
6、ateforanundermaduatelaboratow.lheheartofourapparatusisbasedontherevolutionaryvacuumH-tubereactordescribedbvWavdaandDyein1985(2).Ourreactor,thatwerefertoasabridge,isavac-uum-tightvesselthathastwoormoreseparatecompart-ments.Theentirebridgeisconnecteddirectlytothevac-uumlinebvmeansofastandar
7、dmound-elass"iointthatisassociatedUwiththemainstopco&.Alternatively,theves-selmavbemodifiedreadilvtoenableconnectiontoavac-Figure1.Photographofatypicaltdple-compartmentbridge,fineduumlinethroughtheuseofflexiblestainlesssteeltubingwithtwo100-mLreactionbulbsanda5-mmNM
