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"FesterlyticHydrogenation"byBozakium
[BacktotheChemistryArchive]

35()$&(
Asthoseofyouwhohavebeenfollowingthechemscenethisyearknow,thenewbookfromUncleFesterhasbeen
promisedandpromisedbyLoompanicssinceMarchorsoofthisyear,withthereleasedatecontinuallybeingpushedback,
despitethewordthatitwas"attheprinter's"inJune.Ihavebeenprivytothemanuscriptofavery,dareIsay,
revoloutionarychapterofthisbooksincemuchearlierthisyear,andoutofrespectfortheauthor'sneedtomakealiving,
notdivulgedany"tradesecrets"thoughIhavetoldofsaidformula'smostvitalelement,andteasedofthesimplicitythis
newFesterMethod.
Nowseveralmonthslater,andnearlyayearsincethebookwaswrittenitisstillnotavailableandwearenowtoldby'Panics
toexpectitinSeptembersometime.Yeah,right(sarcasmherefolks).Anyway,whilediscussingthiswithFester,I
mentionedhowIhadteasedtheswarmwithhintsofthenewmethod,buthadn'tdivulgedany"tradesecrets".The
embitteredFester,pissedatthegravellyhandjobLoompanicshasbeengivinghim(allegedlyduetomanagementchanges
orsomething)defiantlytrumpeted"DivulgeTradeSecrets!"InearlybustedatnutwithbothexcitementandreliefthatI
couldnowsharethisbreakthroughwithyou,thescientificworld.Myshiteatinggrinstillaglow,Uncleexcitedlygavemetwo
newreferenceswhichpromisetosignificantlyshortenreactiontime.Itisnowmygreathonortosharethisknowlegeinthe
interestofthefurthermentofscience.Enjoy.
Bozakium1998

$%675$&7
Reductionofthehydroxylgroupofvarious1phenyl2aminopropanolsandtheirsubstitutedaminovariantsareeasilyand
efficientlycarriedoutbyelectrocatalytichydrogenationoftheirrespectiveaceticestersatapalladiumorpalladiumplated
electrodeinadividedelectrolyticcell.Useofalamb'sskinprophylacticasaninexpensiveyeteffectivecelldividerisalso
demonstratedinthisexperiment.

0$7(5,$/6
One(1)gramofpurifiedephedrine,pseudoephedrineorphenylpropanolamine.
Onetroyounceingotofpalladium
Glacialaceticacid
Concentratedsulfuricacid
Sodiumhydroxide
AnhydrousHClgassource
pHindicatingpaper
Toluene
KlingTiteNaturalambbrandcondoms
Leadorgraphiteelectrode1/2inchwidebyfiveincheslong
Sixoneinchalligatorclips
Severalfeetof16to20gaugeinsulatedcopperwire
VariableDCpowersupply
Ammetercapableofmeasuringupto3amps,withresoloutionto1/10ofanamp
Voltmeter(optional)

352&('85(
Onegramofephedrine,pseudoephedrineorPPAhydrochlorideisplacedinalargetesttubealongwith57mLofglacial
aceticacid.Thetesttubeisheatedinawaterbathuntilalltheephedrine(inthiscase)hydrochlorideisdissolved.Afew
dropsofconcentratedsulfuricacidareadded.MixitalltogetherandLOOSELYstoppertheendofthetesttubetoprevent
steamfromentering.Heatthewaterbathtojustaboutboiling,anduseittoheatthetesttubeanditscontentsforafew
hours.Thisformstheaceticesteroftheephedrine,pseudoephedrineorPPAusedinthereaction.
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Thesolutionshouldappearclearandwaterlike,completelyhomogenous.Afterheating,thereactionmixturecanbekept
stopperedasisforafewdays,butit'sbesttouseitimmediatelyafterit'scooked.
Next,mixupasolutionof5mLofconcentratedsulfuricacidin100mLofwater.Takea250mLbeaker,andplaceitona
magneticstirrer.ClipawellscrubbedKlingTiteNaturalambcondominonesideofthebeaker,andplaceapieceoflead1/2
inchindiameterandafewicheslonginsidethecondom.Ontheothersideofthebeaker,standupaoneounceingotof
palladium.Usingalligatorclips,makecontactwiththeingot,andwththepieceoflead.Theyareyourtwoelectrodes.Next,
pourmostofthedilutesulfuricacidsolutionintothebeaker.Saveenoughthatsomecanbepouredintothecondomsothat
thesolutionlevelsareaboutequalinsidethecondomandthebeaker.Theingotofpalladiumshouldbealmostcompletely
immersed.Thealligatorclipshouldbeupoutofthesolution,andthereshouldbeenoughspacelefttoaddtheesterreaction
mixturefromthetesttubetotebeakerwithoutcausingthesolutionleveltoreachthealligatorclip.
Thesurfaceofthepalladiumingotshouldbelightlysandedpriortouse.Thisincreasesitssurfaceareaalittleandexposes
fresh,cleanmetal.Thepieceofleadshouldbescrubbedfreeofgreaseanddirt.Thewireleadtothepalladiumingotcanbe
clippedtothesideofthebeakerwithaclothespinorpapercliptopreventtheingotfromfallingoverduringthecourseof
thereaction.ADCcurrentmeter(ammeter)shouldbeputinserieswiththewiring.AgoodonecanbehadatRadioShack
forunder$50.00.
ThewiresarefirsthookedupsothatthepalladiumingotisconnectedtothepositivepoleoftheDCpowersupply,andthe
pieceofleadtothenegative.Thetypicaloneounceingotwillhaveafacewithanareaofaboutsixsquarecentimeters
immersedinthesolutionandonesquarecentimeterupoutofthesolutuion.Onlycounttheareaonthesidefacingthelead
piece.Thebacksidedoesn'tcountbecausesignificantcurrentdoesn'treachit.Withthistypicalingotapplyabouttwoamps
for30secondstooneminute.Oxygenwillbubblefreelyfromtheingot,andhydrogenfromthepieceoflead.Blackeningwill
benotedontheedgesoftheingot,wherethecurrentismostintense,andalighterdiscolorationontheflatfaceofthe
ingot.Thispretreatmentiscalledanodizing.Ithasbeenfoundthatanodizingincreasestheabilityofthepalladiumingotto
adsorbhydrogenwhenthewiringisturnedaround,andtheingotismadethecathode.
Next,redothewiringsothatthepalladiumingotisattachedtothenegativepoleoftheDCpowersupply,andthepieceof
leadtothepositive.Turnthejuicebackonandrunbetweenoneandtwoampsofcurrentforabout20minutes.Atfirst,
theamountofhydrogengeneratedatthepalladiumingotwillappearsmall.ThisisbecausethePdadsorbshydrogensowell.
Afteraboutfiveminutesofcurrentpassage,thewholesurfaceoftheingotwillfreelybubbleoffhydrogen.
Afterthe20minutechargingwithhydrogen,beginmagneticstirringofthesolution,andpourinabouthalfoftheester
reactionmixturefromthelargetesttube.Adjustthecurrentflowfromthevariablepowersupplysothatacurrentofabout
50milliampspersquarecentimeterofpalladiumsurfaceflows.Ifonehasaboutsixsquarecentimetersoftheingotfacing
thepieceofleadimmersedinthesolution,acurrentofabout300milliampsiscalledfor.Thiswillresultinsomegassingoff
ofhydrogenfromtheedgesoftheingot,butovertherestofitssurfacethehydrogenwillreactbeforeitbubblesoff.The
leadanodewillformabrownlayerofleadoxide,andwillnotdissolveatallinthesulfuricacidsolution.Somesurface
particleswillbekickedofftheleadwhenit'sfirstcharging,buttheydon'tmakeitthroughthecondom.Theleadanodecan
bereplacewithapieceofplatinumifdesired,butleadisalotcheaper.Graphiteisamotherpossibilty.
Keepaneyeonthecurrentmeter,asthecurrentflowcanchangeasthereactionprogresses.Keepthecurrentflowaround
300mA(0.3amp)forthesizeingotgiveninthisexample.When1000coulombs(acoulombisaunitofchargeequalling
oneampsecond)havepassedintothesolution,addtheotherhalfoftheesterreactionmixturefromthetesttube.,and
continueat300milliampsuntil3000coulombshavepassedthroughthesolution.Letususethe300mAcurrenttoshow
anexampleofthesecalculations:At300milliamps,1000coulombspassin1000/0.3Amps=3333seconds,oralittle
underonehour.3000coulombspassin10,000seconds,ortwohours,45minutes.
3000coulombspergramoffeedmaterialhasbeenfoundtogivegoodyieldsofafineproduct,butbynomeansconsider
thisnumbertobeoptimal.Itmaywellbethatagreateryieldwouldbeobtainedbypassingmorecurrent.Itmayalsobe
thatpseudoephedrineandPPAdifferfromephedrineintheireaseofelectrocatalytidhydrogenation.Idon'tthinkthatany
harmcancomefrompassingmorecurrent,withinreasonablelimits,sobyallmeansexperimentwiththeamountof
currentpassed.
Duringthecourseofthireduction,thecolorslowlychangesfromitsinitiallyclearcolortoslightlytintedwithyellow.It'snot
knownwhetherthiscolorchangeisduetosomeofthecondomsoakingout,orifit'sabyproductofthereaction.Inany
case,it'saremarkablycleanreaction.
Whenthedesiredamountofcurrenthaspassed,theworkupandisolationoftheproductisverysimple.TheKlingTite
condomisremovedfromthebeaker.afterpullingout(nopunintended)theleadelectrode,thejimmyhatis,asiscustom
insomeparts,flusheddownthetoilet.Theanodecanbeusedoverandover.Thepalladiumcathodeisthenrmovedand
rinsedoff.IttoocanbereusedanINNUMERABLE(Bozakium'semphasis)numberoftimes.Theprocessofanodizingthe
palladiumwillhavetoberepeatedpriortoeachrun.Somefreshmetalmayhavetobeexposedonoccasionbylightsanding
ofthemetalsurface.Aningotofpalladiumshouldlastforalifetime.
Thereactionmixtureshouldbepouredintoasepfunnel,anda20%NaOHsolutionshouldbeaddedwithshakinguntilthe
solutionisstrongly(13+pH)alkalinetopHpaper.
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Extractwithtwo50to100mLportionsoftoluene.Thisshouldbeplentyforonegramofproduct.THetolueneextractsare
thenbubbledwithdryHCltogetthecrystallinehydrochlorideproduct.Afterrinsingthemoffwithsomefreshtoluene,they
arespreadouttodry.
Themostpleasantlysurprisingfindingisthatcrankproducedbythismethoddoesn'tgiveonethebodyandsoulwrenching
hangoverssotypicaloftheproductmadebytheiodineredphosphorousmethod..Thisisahighlydesirablewaytokeep
one'sownpartyrockingandrolling.
Ifoneshouldwishtoproducemorethanagramorsoatatime,alargerpalladiumcathodeshouldbeused.Linkingtogether
moreingotsofpalladiumwouldgetprettyexpensive,soamoreeconomicalalternativewillbedetailed.Thatalternativeis
electroplatingsomecopperorbrassscreenwithathickcoatingofpalladium.
Thesimplestwaytogetthissectionofscreenelectroplatedwithpalladiumistogototheyellowpages,lookunder
electroplatersandfindonewhoplatespalladium.Askforaplatebuildupofseveralthousandthsofaninch,sothatenough
Pdisdepositedtolastawhile.
ThePdplatedscreenwouldthenbeusedexactlyliketheingot.Firstitmustbeanodized,thenchargedupwithhydrogenin
exactlythesameway.Thesoledifferenceisthatthegreatersurfaceareaofthescreenfacingthecondomencasedanode
requiresacorrespondinglygreateramountofcurrenttobepassed.Then,duringthecourseofthereduction,again50
milliampspersquarecentimeterofsurfaceareafacingtheanodeisused.Thetotalof3000orsocoulombspergramoffeed
materialdoesn'tchangebyincreasingthesizeoftheelectrode.
Analternativetothisisplatingthescreenyourself,anodicallydissolvingaportionoftheingottoformaPdCl2solution
then.....sorryfolks,thisallofthemanuscriptIhave,butI'msurepalladiumplatingisnonationalsecret(yet).
Thereisacompanythatsellsanelectroplatingkitconsisitinofapowersupply,metalsolutionanda'pen'electrode.Assoon
asIfindtheirpaperworkamongmyrubbleIwillpostit.
ThelastestwordfromFesterisacoupleofreferencesfromIndianjournalsonelectroplatinggraphiteelectrodeswith
palladium,essentiallygivingaPdblackonCcatalystinthecell!
1)Krishnan,ElectrochemicaActa,Vol21,Pg449450(1976)
OntheElectrochemicalReductionofBenzylCyanidetoPhenethylaminewithaPd/CElectrode(note:Thetitlemaynotbe
exactduetotheillegibilityofmychickenscratchtranscriptionofmyconversationwithUF.)
2)Krishnan,JournalofAppliedChemistry,Vol5,Pg125128(1975)
ThegreateractivityofPdonC(overstraightPd)resultsinashorterreactiontime.
Ifanyonemanagestofindthesereferences,pleasepostthematthehive.I'dalsobehappytoansweranyone'eelectrical
questions,aslongasyouarenotdoinganythingillegalofcourse.Enjoy.
AddendumbyReadyeddie:
Rhodium,Ithinkyouneedtochangesomethingonthefesterformulaonyoursite.Theproblemistheesteritsaysaddhalf
ofitthenwait45minorsothenaddtheotherhalf.Witchiswrongbecauseagramneeds3000coulombstobepassed.If
youaddtheesterintwopartsitwillleavehalfoftheproductunreacted.Whybecausethesecondhalfwillnothavetheright
amountoftimetobehydrogenated.Witchwillgiveamixofmethandstartingfeed.Theestershouldbeaddedallatone
timeandranuntil3000coulombshaspassed.Butontheotherhandsomepeoplethinkwhynotjustrunlongertoletthe
secondhalfhavetherightamountoftimetoreact.Wrongwhybecausethefirsthalfoftheesterwillmoreandlikelybe
changedbacktothestartingfeed.Justtryingtohelpotherwhereothershavefailed.

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