Swim found iss
This began as a reply to cheese's tone still prob but developed into this. Thought it needed it's own space
Semi Orginized Notes On Efficent High Quailty
Amine Jewlrey Production
If you cant get the tone to come over under vac. try this. Run the oxone buffered from the start.if the rxn goes over 40.c it will without a doubt be overoxidised. adding a little dcm to the alkene with the oxone will maintain a decent temp if the rxn goes exo on you. that is the problem with scaling this up. the exo shit will fuck you every time. the distilled overoxidation product is clear yellow carries a distinct safroley flower aroma kind of sickning after a while and it will freeze after sitting in the freezer for a while. the B.P is bout half between the tone and alkene. Super shafty rxn temp max of 53.c yeilds 95+/-% of this supershafty worthles shit. when this compound is subjected to H2SO4 rearrangement and thermal rearrangement it yeilds a product that jells before it freezes.It carries a similar uv color to ketone but just a little lighter. SMells strongly of very burnt goodyear tires extract 2x with dcm combine exrtacts and wash them with 5%NaOHx2 then bicarbx2. The washes are removing the small ammounts of pheonilic compounds. do your reflux with the H2SO4 15% make sure you check the density of the H2SO4 solution prior to use. run it with a plate temp of 100 which will provide an internal temp of the required 80.c and employ stirring sufficent only to maintain a fine suspension of Ca. .5mm beads. at 2.5Hrs hit it with a chunck of distilled ice and carefully and quickly neutralize with bicarb. hit it twicw withthe dcm repeat the NaOh Bicarb washes as done with the epoxide. still the dcm. Then if you got it hit it on the outside of the flask with liquid N2. any unreacted alkene or overoxidation shit will xtylize quickly pour through a scotchbrite pad imediatly followed by a small piece of dcm. shit should bee looking pretty clean now already. PLace crude ketone/possibly some unrected epoxide in 2xoversized rbf with an vertical air condensor/collum ->head->vac adapet->recieving flask. set the stillin flask in a Jr.Fry Daddy in peanut oil that has been preheated to max temp. as soon as the dcm comes out then attach the collum/assembly. ass soon as the temp in the flask is at max for a few minutes then slowly and carefully apply full vac to attain vigerous boiling to the point of the shit traveling up the collum and into the recieving flask. Do it under UV . you should only have tone/pox/shafty shit in there. keep a sample of the pox prior to rearrangement to compare uv color. the tone will be a lighter shade of clear green than the pox that will be a darker green. twards the end you can see the drops of darker shit hit the recieving flask. as soon as this happens kill the vac and let tit run at full temp for a 15-20 mins minutes. here one of two things will happen, depending on how effective the predistillation washing went. if you did it shafty like what is left will rearrange to tone then rapidly polymerize. If you did a quailty job then it will still be very fluid as soo when it is hit again with full vac the rest will come out as ketone leaving only a small ammount of shit in the flask. Decent levels of purity can be attained through diligent washing and this distillation technique the bulk of the tone must be removed very rapidly with the vac if the alkene/over shit was froze out proper than the tone will be the first fraction to come over. if it is going too fast and you see dark shit at the base of the collum then let off on the vac slightly and let it fall back into the flask then crank it down again if you over shoot it and accidently let too much epoxide get through. then set it back in the frydaddy under reflux for a 20 mins or so. so long as there isn't brown shit in there most likely it wont polymerize through a second heating to get the last of the shit to convert. Also a heafty drying of the ketone might help withteh amination. why don't you use an Nitro Al/Hg until you get the tone how you want it. no sense to waste expensive shit. Use excess Al. Add all the nitro and let it react before adding the tone. begin tone drip when the internal temp is down to 45 or so. EtOh can be found that is denature only with MeOH OTC they work great and can be had by rthe gallon for cheap. Kind of shafty getting OTC MeOH in the summer. when the nitro is added first ass soon as the tone hits the rxn it quickly forms the imine and gets reduced leaving little oppourtunity for side rxn to occur. also the rxn will not be as hot when the tone is added=more meAm in solution. When back to room temp remove condensoe and attach a thermo adapter with a non collapsable tube to the top of the flask and run that into the bottom of a container of HCLattach the vac to the top of that container and pull a vac high enough to pull all excess MeAm out but not enough to bring out the solvent. Reuse HCl for this until PH is nuetral at which point adjust to 40%aq MeAm to use in bigger reducts when it is done you'll be ready for it. If ya don't got a variable vac then get one.
Xtal preperation- not the most efficent but damn accurate. no eating up of the shit.
Me am has already been took by the vac/hcl so solution don't smell too shafty. Pour through scotchbrite pad to remove excess Al chuncks then basify slowly with 35%naOh just a small ammount enough just to make tiny clear bubbles in the grey supernat let sit for 20-30 mins at which time the sludge will have dissociated a bit and pour it through a 2xstack of scotchbrite pads then pour your tolly through the funnel/pads and add a tiny bit more NaOH spin for a few minutes then seperate. it will sep fairly quick load some drying agent into the funnel now and pour the tolly/basefreebase throughthe drying funnel and gas. when xtyls are all out add sufficent water to digest all xtyls. sep wash with toul leave it there add some boilind chips and set plate to 100 and hold iut there for a few minutes. pour off toul allow to cool and basify again.extract into as smaller ammount of toul than with the first extraction from the reduction. dry gas again. filter wash with Dry/Cold tone. then dissolve xtyls in minumum boiling dry IPA. shouldn't be anything to filter but if there is then do it while hot. Set the temp safe dishin a vessel of ice and wait till it i sall out and pour the alcoholoff. then make up a slightly smaller ammount of dry ipa tha used in previous rundissolve the xtyls again while boiling but this time have the lid to the dish up side down with ice in it as to not let the ipa boil out slowly adjust the temp down over the period of a few hours slowly tuhning the plate down. let sit at room temp for a couple more hrs then set it in a mess of ice water for an hr then the freezer for an hour. Diamond Ice yummy tummy chuncks dadadadamn and from such a slappy tone stillin. Take ice diamond yummy to jewler and have set into a heart pendant.
Bet ya didn't expect that
Vl_