Author Topic: why iso..??  (Read 17837 times)

0 Members and 1 Guest are viewing this topic.

tina_craig

  • Guest
Workin' it again.
« Reply #60 on: October 12, 2004, 03:41:00 AM »
4 boxes of 24 x 30 pills super loaded with inactives were first put into a "beaker" and covered with acetone until about 1/2" of tone stood over pills.  Then dh20 was added 4-5 drops at a time and then swirled.  This was repeated in these increments until red began to losen and was finally removed to a slight orange tint.  Pills then filtered and allowed to dry overnight.  Then crushed to a fine powder in a "mortar and pestle" and covered with 200ml of 91% ISO IPA and allowed to sit 24 hours.  Then filtered and put over heat, as small bubbles began to move quickly from bottom to top of alky, 12 grams of KOH chips were added in 4 gram increments over about 15 minutes.  Then solution was boiled 30 minutes.  Color changed from red-orange to melon to milky white with coffee colored layer on bottom.  This has been allowed to sit 24 hours to settle and is awaiting evaporation due to lack of time.  Will post further results as they are obtained.  As of now, solution is almost clear with the coffee layer and now a white layer on top of the coffee.  Will sit at least another 24 hours before evaporating.  Looking very good so far though.


rangahtank

  • Guest
Gassing longer
« Reply #61 on: October 15, 2004, 09:47:00 AM »
Recently, while trying this method, SWIR couldn't seem to get the goodies out of the toluene.  After much head scratching and pondering, he simply 'overgassed' the tolly.  The extended gassing seemed to precipitate the pfed HCl with few gaks following.

SWIR still likes to rextallize twice anyway before reacting, and has noticed few problems with this overgassing.

UncleFester

  • Guest
wasted 'tone
« Reply #62 on: October 15, 2004, 01:03:00 PM »
No need for any solvent presoak except with the 200 mg guifenesin pills with 25 mg ephedrine. Decant off the clear alcohol from the settled flakes and coffee layer, and just proceed with the workup.

tina_craig

  • Guest
Last night, swit_c brought ISOIPA that was...
« Reply #63 on: October 15, 2004, 04:05:00 PM »
Last night, swit_c brought ISOIPA that was holding pseudo after KOH boil from most recent post with the pretty colors to another boil and boiled down to 1/4" of fluid left in beaker.  Lots of sparkly xtals.  Added 20ml of dh20 once completely dry and swirled, added to sep. funnel, added 25ml tolly to beaker, swirled, added to funnel, added 50ml more to beaker swirled added to funnel.  Washed with dh20 3 times.  Drained tolly into clean beaker and let sit overnight to drain entrained water, noticed tolly was perfectly clear this morning.  Water washes remained cloudy. What water couldn't get drained in sep funnel was left with a very small amount of tolly on top.  Gassed this and put in evap dish to find nice crystalline, film this morning that looked kind of like how ice freezes to windows in the winter.  Will gas tolly tonight as was on way to work.


UncleFester

  • Guest
careful with that heating!
« Reply #64 on: October 16, 2004, 02:14:00 PM »
As the alcohol nears being completely evaporated away, one must be careful with the heating on the evaporation. If you heat to dryness, you may well burn the pseudo extract and end up with nothing. Hot water and a fan blowing over the top of the beaker may be the best choice for rapid evaporation of that last bit.

UncleFester

  • Guest
more stuff
« Reply #65 on: October 16, 2004, 11:07:00 PM »
As to the KOH usage, on my first run I tossed in maybe 7 gr per 100 pills and boiled for 15 minutes. To see if there was more to get, I let the layer fall to the bottom and decanted the alcohol. The alcohol went back to the beaker, and I added another gram or so of KOh and boiled for another 10 min. I got a little bit more layer at the bottom. If that was from not allowing enough time for the layer to fall out all the way and settle, or if it was from more gak being whacked, I'm not sure. The brand name pills and most generic knock offs which plug filters certainly benefit from going up to 10 gr per 100 pills. Beyond that, as to increasing time or more KOH, one could repeat my original line of thought by just separating off the precipitated crap and boil more or add some more KOH and see if more crap falls out. I think 10 gr is enough for the pills now out, but do give it a try if you want.

UncleFester

  • Guest
the gassing...
« Reply #66 on: October 16, 2004, 11:12:00 PM »
if I read your posting correctly, all you have is an ice film of psuedo? It should be a snowstorm which requires filtering and drying. Do give more details....

UncleFester

  • Guest
my personal punching bag
« Reply #67 on: October 17, 2004, 01:30:00 AM »
My kids are too nice to whack, but if I did my son would put up a battle. Your posts on this page allow me to be a whacking bastard. The pills require no solvent presoak, but if a presoak should be done, it better be np. Instead you modify the procedure and use acetone and water presoak. Both dissolve product, and both could be used as recrystallization solvent. What buzzing was in your ears after reading the experimentals in the rest of this thread that caused you to do this?? If you have an itch to presoak, use toluene, xylene or naptha.
Then after letting the entrained water in the extract settle, pour into a clean and dry beaker to gas, while leaving the water droplets behind. Don't act like a violated or otherwise misused victim when reading this post because you said previously that you were going to follow the procedure, but continue to invent amateurishly along the way.

tina_craig

  • Guest
the tone and water was only used because swim...
« Reply #68 on: October 17, 2004, 09:40:00 AM »
the tone and water was only used because swim was told to at least remove some of the red.  The ice film swim spoke of was from the tiny bit of water and tolly that swim couldn't separate do to ghetto sep.funnel, so swim figured what the hell and evapped that little bit while waiting to gass tolly.  When finally gassed it gassed beautifully, returned about 2 grams.  Swim reacted this with 6g I and 4g MBRP (excessive swim knows but got tired of disappointments) and 1ml dh20 inside about a 400-500ml ghetto flask with 4' of braided pvc hose and a punch balloon on the end.  Cooked for 3.5 hours did a standard workup and returned about 1.25 to 1.5 grams of kickass sheite!!  Prepping a 7 grammer with UF's technique on some generic waly's world 60's.  So far so good........and high, woohoo!


UncleFester

  • Guest
citing referenes...
« Reply #69 on: October 18, 2004, 12:10:00 AM »
...for acetone as recrystallization solvent for ephedrine and sudo. There is the Emde article from Chem Abstracts from the '20's that everyone should be familiar with, also Chem Abstracts Vol. 47, col. 3347. Cold acetone can be used as a quick wash, but not a presoak as that uses large volumes of solvent. The stuff dissolves the goods and should be used appropriately. Quit worrying about the color of the coat of the pills, it's what is inside that screws you.

tina_craig

  • Guest
White 60's
« Reply #70 on: October 18, 2004, 04:18:00 PM »
6 boxes of 24 x 60 Wally's world generics listing 3 inactives.  Crushed to fine powder, extracted 3 times with 150ml 91% ISO IPA.  Each 150ml portion brought to a boil separately and added 10g KOH each at time of boiling.  Boiled 30 minutes each.  Allowed these to sit for 30 minutes each to settle, then decanted and combined extracts in evap dish and evapped to near dry.  Scraped xtals from dish and added 30ml dh20 put this in sep funnel, added 75ml of tolly to dish 3 times and added to funnel.  Washed with dh20 3 times with volumes equal to 1/2 volume of tolly.  Poured into clean beaker, allowed to sit 30 minutes to drain entrained water and gassed to recover 6g out of 8.64g total available of very high quality pseudo.  Reacted this and all went like a dream.


Xaja

  • Guest
Hey Fester
« Reply #71 on: October 20, 2004, 12:37:00 AM »
Whats your view on hydrolysing by acid reflux? We know it won't destroy the E but will racemize it (ref = The Alkaloids, Manske etc). Wonder if acid reflux (~10% HCl) will hydrolyse polymers also?


UncleFester

  • Guest
acid hydrolysis experimentals
« Reply #72 on: October 20, 2004, 01:04:00 PM »
They're in the thread a few pages back.

Jacked

  • Guest
color
« Reply #73 on: October 21, 2004, 10:10:00 PM »
UF try taking some of the red off first (WW red dots)(dull finnish) and see how much faster it filters. Its like night and day compared. I would recommend that one step before doing an extraction requiring a filtration..


abominator

  • Guest
This bee tried Jacked's advice on da red one's
« Reply #74 on: October 21, 2004, 10:53:00 PM »
This bee tried Jacked's advice on da red one's and by god he is right again! ;)   De-redding works wonders for the filtration.  With no notice of lost pseudoephedrine.

Here is a link for the sulfuric acid hydrolysis and an excerpt:

The 7% final sulfuric acid concentration run gave maybe 25% yield of what seems to be high quality pseudoephedrine. It may well be mixed with ephedrine, racephedrine...
The 5% final sulfuric acid concentration boil gave over 50%, and maybe close to 65% yield of what seems to be high quality product.





 

Post 523508 (missing)

(UncleFester: "sulfuric acid hydrolysis", Stimulants)




PolytheneSam

  • Guest
Post 172833
« Reply #75 on: October 24, 2004, 03:41:00 AM »

Post 172833 (missing)

(PolytheneSam: "Re: Polymers, polymers: BLAH: Gimmee a BRAKE", Stimulants)



UncleFester

  • Guest
getting the red out
« Reply #76 on: October 24, 2004, 01:39:00 PM »
So that's where they put that filter plugging ingredient. It's just amazing how fast the stuff will make a coffee filter nonfunctional. On the post after the sulfuric acid hydrolysis you will see that after the solvent evaporated from the gassing it became apparent that the product wasn't the good quality material obtained from KOH hydrolysis and would need recrystallization.

thinkpol

  • Guest
KOH
« Reply #77 on: October 24, 2004, 01:39:00 PM »
is the evaporation of KOH from drain cleaner fesible?

Furthermore, from a solution that in its MSDS is described as 16% KOH and the rest comprising of water.. Would such a method be suited?


Amnesia

  • Guest
if its 16% KOH and 84% water, then as your...
« Reply #78 on: October 24, 2004, 03:16:00 PM »
if its 16% KOH and 84% water, then as your name says... THINK.

Evap, so you minus the water... you will be left with just KOH.

Thats ALL the info you gave us, and what i gave you is the only answer you can get back, and of course you could of worked that one out for yourself, no?

And if your asking that question expecting someone to turn around and go, no theirs some denaturant in their, how the hell is anyone suppose to know. Because you said it yourself, its just KOH + Water.

tina_craig

  • Guest
Cause for concern?
« Reply #79 on: October 25, 2004, 04:04:00 PM »
2 questions.  1. Last KOH boil developed 2 layers but lower layer remained clear to milky, pseudo gassed from tolly as usual and appears fine, should no coffee color in bottom layer bee a concern? and 2. Can KOH used in this process bee recycled and if so how?  Take it easy on swim UF. ;)