Vibrating_Lights (Hive Addict)
05-21-02 20:34
No 311995
      Amine jewlrey  Bookmark   

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               wink     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 thattongueVl_
 
 
 
 
    Rhodium
(Chief Bee)
05-21-02 20:51
No 312014
      Could you please rephrase the post WITH some ...  Bookmark   

Could you please rephrase the post WITH some punctuation. I cannot read this.
 
 
 
 
    pickler
(Greenhorn)
05-21-02 22:21
No 312065
      overoxidation  Bookmark   

reffering to



Run the oxone buffered from the start.if the rxn goes over 40.c it will without  a doubt be overoxidised. that is the problem with scaling this up.



Exactly how far are you scaling this up to have to deal with the overoxidation?

We'll soon find out if I'm a chemist or not!
 
 
 
 
    Vibrating_Lights
(Hive Addict)
05-21-02 22:52
No 312087
      Sure  Bookmark   

It is going to take a while. No numbers will be included.  Swim will Make up a Cost Per Mole. Swim has found that using punctuation when writing something this long lately interfears with thought proscesses for some reason.Probably lack of sleep in general. Using these techniques one could expect to get 9.75 gms of salt per 25gms 2 alkene or 30 gms of 1 alkene conversion of 1 alkene is near quantative no forrun last bit is left in designated iso flask Jtbaker KOH Pellets  are ground into a powder.
Rxn can be scaled indefinatly employing a bar visable stirring vortex. With temp kept under control.
VL_
 
 
 
 
    psychokitty
()
05-28-02 21:24
No 315277
      Here 's your oxone/AA solubility information
(Rated as: excellent)
 Bookmark   

20 parts acetic acid in 50 parts d-water dissolves very easily 7 parts oxone; there is a precipitation of some unknown substance.  Addition of 20 more parts of acetic acid does not affect solubility of precipitate.

20 parts of methyl alcohol in 50 parts of d-water dissolves 7 parts of oxone as per usual; standard precipitation occurs.  Addition of 20 parts of acetic acid does not change the precipitate distribution much; however, it does change its composition slightly and is accompanied by much fizzing and popping (presumably through sodium carbonate reaction with the acetic acid).

20 parts of acetic acid and 7 parts of oxone yields a precipitate that when filtered weighs approximately 3 parts.  This solution is considerably easier to stir that standard alcohol/oxone mixtures.  Addition of 20 parts more oxone and later 20 parts d-water does not affect the appearance of the precipitate.

Conclusion:  Acetic acid may be a better solvent than methanol for the oxone reaction (or a combination of both).  No isoalkene was used in these experiments.  These results may pave a way to a better perepoxidation or perglycolization as the acetic acid may react with the sodium carbonate found in commercial oxone samples to yield sodium acetate which might serve to buffer the acid oxone reaction and thereby increase yields of the glycol product (which are normally quite low using the standard unbuffered oxone reaction).  Futhermore, acetic acid may serve to better solubilize the isoalkene during the reaction and allow for a decreased initial reaction temperature which may also increase yields.
 
 
 
 
    Vibrating_Lights
(Hive Addict)
05-29-02 06:13
No 315468
      thank you much  Bookmark   

Thanks much. Thats the kind of info we need.
Vl_
 
 
 
 
    cheeseboy
(I'm not Cheesie)
05-29-02 21:38
No 315709
      %?  Bookmark   

Vinegar, or like the strong % acetic acid shit  (AA)Never used it, that's why cheese don't know much about AA

- "Start at the TOP, because shit runs downhill."
       - the Plumber
 
 
 
 
    cheeseboy
(I'm not Cheesie)
05-30-02 21:14
No 316015
      vinegar  Bookmark   

Hey psychokitty, does the acetic acid have to be of the 80% shit or can one use plain vinegar instead of methanol?


- "Start at the TOP, because shit runs downhill."
       - the Plumber
 
 
 
 
    humidbeing
(Can't SWIM)
05-31-02 20:00
No 316354
      acetic  Bookmark   

Is,nt acetic acid distilled out of vineger anyway?
Shouldn't be hard to make your own.
Chemfinder gives the Bp as 117.9 and the Mp as 16.6.
What is the acid content of the strongest vineger you
can get?
Hell, just buy it at photo shop.

CG I miss you sweety, I really do.
 
 
 
 
    cheeseboy
(I'm not Cheesie)
06-01-02 03:20
No 316491
      ya>?  Bookmark   

Well apparantly plain 'ol vinegar wont do the job right. Too much water being used. Oh well, who wants to get good yields of the Diol anyhow. Thanks for the info..

Bubba Fatt - LA's Biggest Bounty Hunter. His subjects are at large and so is HE!

Edit in:  Also cheese tried using a tightly knitted wool sock to add the oxone powder, this way there's not tedious filtering. All you do is weigh out your oxone and dump it into the sock, then just combine your methanol & dH2O then just dunk the sock in. Takes about 5 minutes of swirling and squeezing the sock for all the oxone to be digested and you are left with the potassium salt left in the sock. Tea bag approach.smile
 
 
 
 
    Vibrating_Lights
(Hive Addict)
06-01-02 06:53
No 316562
      teabag?  Bookmark   

That teabag sit is awesom.  did you get approiate yeilds when adding this way? Oxone is too tedious to filter through a funnel. To get GAA from vinigar neutralize with bicarb then evap to obtain Sodium acetate.  add with H2S04  under ice bath and distill ou the gaa.
VL_
 
 
 
 
    cheeseboy
(I'm not Cheesie)
06-01-02 23:43
No 316746
      Cool  Bookmark   

Thanks VL_ that explains it. Phew., well prolly just fuck the GAA thing. I hate Vinegar on anything else than fries and gravy . (fries and gravy with vinegar RULES!)

Bubba Fatt - LA's Biggest Bounty Hunter. His subjects are at large and so is HE!
 
 
 
 
    Vibrating_Lights
(Hive Addict)
06-02-02 03:22
No 316789
      teabag  Bookmark   

Tell me about the fucking tea bag god damn it.Fear and Lothing