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TheOnePotd,lMethandICE.
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LaBTop..........posted06239901:04PM
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Makingofd,lMethice(cream).
Ingredients:
138gramP2P=+/1grammole.
1000mlMethanol(+10%weightMethylaminegas)=+/3gmol.
36gramMgSO4.7H2O(dryat300Cfor2HrsinoventogetMgSO4.1H2O)=toattrack2gmolH2O.
200mlSilicagelballs+/3to5mm(dryat300Cfor2Hrsinoven,changestodarkbrown!).
15gramNaBH4asareducingagentfortheformed(waterfree!)Imine.
IMPORTANT:THEREACTIONISVERYSENSIBLEFORANYWATER(fluidorvapourintheair!).
FirstquicklycrunchyourDRYMgSO4toapowderinamortar,anddirectlyputthatundermax.mixinginthe
Methanol/M.A.mixandclosethepottoletnowaterfromtheairin.Keepmixingfor10minutes,thenallthewaterwill
betakenuptotheMgSO4.LetstandandwaittillalltheMgSO4isonthebottom.NowquicklytapoffthenowDRY
MeOH/MAmixin2Lreactionflaskandclosethatone.Washdirectlyyouremptypotwithlotsofwater,toremovethe
smellofmethylamine!Nowaddthe200mlDRYSilicagelballsandamagneticmixerbaralsointheflaskandclose
again.Keep2LflaskinSiliconeoilbathat20C.Siliconeoilonlyslowlywarmsup!NowaddSLOWLYviaa
droppingfunnelthe138grP2Ptothe2Lflaskunderstrongmixing.Thetemperaturerisesto23Cduringthewaterfree
Imineforming.ThewaterfromthisreactionistakenupbythedriedSilicagel!Thistakes30minutes.Letthenmixfor
another1hour.Thereactionmixcolorchangesfromlightyellowtocoffee+milkcolor.Temp=23C.Stopmixingafter
this1hourandpourthefluidoffintoa2Lglaserlenmeyerwithflatbottomandaddamixbar.TheremainingSilicagel
iswashed3timeswith50mlDRYmethanol,tocatchtheremainingImine,andthose2x50mlisalsopouredintothe
2Lerlenmeyer.Nowputthe2Lemonmagn.mixer,inaicecubes/methanolbathandstartstrongmixing.PutaFunnel
ontopof2Lem,inrubberring.Nowstartadding,every5min.,ateaspoonfull(flatoff!)ofboroandwashinwith
minimummethanol.Aftereveryspoonfull,stopperthefunnellooselywitharubberstopper.Thistakes2,5hrs.DO
NOTexceedatempofmorethen20C!!Youcanaddthenextspoonat+/8C.Solutioncolorislightclear
orange/brown.Letmixintotalfor8,5hrs.(couldperhapsbelotlesshours,do'ntwanttoknow:timeisNOTmoney!)
Thetotalvolumeis+/1900ml.Addthenthemixto5Ldest.waterina10Lflask,undermagn.mixing.ThepH=12.
Addthen500mldiChloromethane(DCM)andmixstronglyfor30min.Letoilprecipitateandadark,honeycoloured
layerofDCM+oilisonthebottom.Decantthewaterpartwithaaspirator+siliconetube.Filltherest(water+DCM+oil)
inaseperatorfunnelandtapoffonlytheDCM+oil=550ml.(DCMboilingpoint=40C).TheleftoverMgSO4andboro
saltsstayednicelyinthewaterpart.ThendrytheDCM+oilwithsomeDRYMgSO4anddecantin2Lem.Washthis
MgSO4withsomefresh,DRYDCMandaddtheDCMwashingstothenowdryDCM+oil.TotalvolumeDCM+oil
=1000ml,colourishoney/red.Startnowbubblingthis1000mlwithHClgas,while2Lemstandsinicebathon
magn.mixerandmixstrongly.CheckpHfrequently,untilpH6.Pourthenowacidified1000mlina2Levap.flaskand
putonRotavapmachine.Speed=100rpm,temp=80C,mode=p/auto,littlevacuum=800mbar,toholdtheflask.After
distillatingoffnearlyalltheDCM,suddenlythecontentsoftheflaskturnsfromdarkhoneycolourtocreamymilk
coloranditdriesouttoaroundcakeonthebottom.Removethe1LDCM,nowinthecollectorflask,andhangthat
emptyflaskonagain.Nowputfullvacuumontoremovethelasttracesofwater.Cleaningby3xrecrystalization:Put
MINIMUMquantityofhot(40C)DRYDCM(ordry98+%Ethanol)intheflaskuntilthelastremainsofthedrystuff
dissolves,andadd4xthisDCMquantityasDRYacetone.Closewithstopperandput1hrinfreezer.Asoliddirty
whitecrystalmassisformedwithalayerofdarkredfluidontopofit.Decantthefluidandrepeatthisstepanother2x
and2Hrs.Youhave,thelasttime,snowwhitecrystals.DryWeight=141,5gram,closetoquantitativeyield.Youcan
eventuallymeltthiscrystalmassinaaluflatbottompotonaheaterplateat170175C.ThenletthismeltVERY
SLOWLY,anddonotgohigherthennecessarytomeltit,oritsstartssmoking(youhaveyourfirstquicktestthen:
enjoy!).Cooldownto150Cagain,reallyslowly,1degreeCper30min.(regulatewithyourtempcontroller!),andyou
gotd,lICE,afteryouletitveryslowlyagaincooldowntoroomtemperature(withaclosedlidonit!,itshygroscopic!).
Advantage:youremovedALLthewaterinthisprocess!!!
SonowyouknowatlasthowtomakeICEcream.......RaversLOVEit!!!! LT/
EMOTIONSwillalwaysbeFREE!
LaBTop..........posted06239901:19PM
Member
Yohoo,forgottotell:
UsedTartaricacidtogetdMeth!!!!!!!!
2Fliesinonehit....
Askyourbelovedmoderator,theunforgettableMRSpit_tartar_Ball,howtodothat,herecentlypostedthemethod,but
needsalittleexplainingformostofyou,I'mafraid.ButthoushouldNOTbeafraid,itseasy!
ThenyouhavedMethANDlMeth(speedyonly).Lifebecomeseasierandeasier......? LT/
