KOH Pseudoephedrine Extraction (Original procedure by U.F.)

tina_craig · Tue Feb 08, 2005 9:41 pm

Pseudoephedrine HCl
KOH Hydrolysis by swiUncleFester
2.88 grams available pseudoephedrine HCl
10 grams 99.9% KOH (Potassium Hydroxide)
200ml-300ml 91% Isopropyl Alcohol
dh2o
toluene
HCl gas generator (37% Hydrochloric Acid and Calcium Chloride)

Dered if necessary, grind pills to fine powder. Cover with ISO IPA, shake and let sit about 1 hour with shaking every 15 minutes or so. Filter through fine filtration (ie, charmin plug) into heat safe glass container (beaker, flask, switc uses a coffee pot for a nice BIG beaker). Bring to near boiling, add KOH slowly. Boil 30 minutes. Allow to cool and settle in separatory funnel. Upper layer should be clear to white. Drain lower layer. Drain upper layer into evap dish. Evaporate on low heat with a fan. When evapped pour 20ml dh2o into dish put this in sep. funnel, add 75ml of toluene to evap dish and get all crystals, add this to sep. funnel. Wash 2x with dh2o draining h2o layer each time. Filter toluene through dried epsom salts and gas, should yield 70% of pseudoephedrine HCl, continue with 1-2 recrystallizations.

beaker · Busy Bee

Thanks TC, I pm'd someone for this exact write-up and it was suggested that I buy the book.

java · Consumer

uncle.fester
Master Deconstructionist
Posted - Feb 09 2005 : 12:04:23 AM

Now I am just passing along scuttlebutt, because I would never dream of checking out pill formulations...but this is what I have been told...
It seems that over the past 6 months or so, the gak loading of generic **** and generic **** has been increased since the last time they were checked into. It takes roughly 15 gr of KOH per 100 30 mg pills to cut through them, and the oily layer and flake layer is larger. Also, the alcohol layer doesn't become clear as before, it retains a slight melon tint.
It also may well be that the product has an affinity for this oil layer and could be lost there...somebody should check into recovery techniques.
Another point is that during the KOH boil, if the alky evaporates away enough, it could aggravate the problem with losses into the oil layer...another recovery technique investigation for brave experimenters...or just add more alky during the boil to maintain volume.
The bottom line on these generics sited by ****** is that the gak load has gone up much in the past 6 months or so

............as posted at WD by Uncle Fester

tk3god · Tue Feb 22, 2005 9:33 am

this may be an obvious question but with 99%ipa can one just add 8% dh2o for 91%?

tina_craig · Wed Feb 23, 2005 7:47 pm

THE MOON RULES --1 · voted for the moon

Correct me if I'm worng. I've never made dl-"N,alpha-dimethylbenzeneethanamine hydrochloride" or done it for that matter but from reading rhodiums site doesn't the straight to e, extraction seem the easiest and most OTC?

stooge · Fri Feb 25, 2005 7:22 pm

ahm, do i get this right, would this also work with pills with Macrogol and Antihistamins or is this only usable for pfed-only pills with gak ... ?

loki · guinea pig

i discovered some weeks ago that pills can be readily caused to break apart by irradiating them with microwaves in a small amount of water. i've posted a thread about the idea of doing the same thing in xylene or something similar - the key point is that if you don't add water, then you don't get troubles.

the microwaves, in the hypothetical scenario, sitting in xylene/toluene in the microwave, penetrate into the pills directly and cause the water inside them to expand vigourously. no water around them makes this more pronounced (in theory). once they are thoroughly broken apart this way, the nonpolar solvent soaks up waxes and vegetable oils etc.

the idea was to follow this with 3 boils each of naptha and then dry acetone, and a chlorinated hydrocarbon has been suggested as well

If these gaks are annoying in ways similar to povidone (another polymer used in pills) then they probably share some characteristics, such as being insoluble in the nonpolars... take heart, povidone is soluble in chlorinated hydrocarbons and in ketones too...

thus, the three boils (or maybe soaks) described would theoretically wipe out many polymers, waxes, oils and gums.

Then, to be a bit different, and probably some folks don't know this but soaps are frequently added to pill formulations, boil in fairly strong HCl solution, maybe 2-5 molar, this will transform all the soapy crap (eg magnesium stearate) into HCl salts and fatty acids (remove them with a nonpolar liquid/liquid extraction). An acid boil may be effective for denaturing some of those nasties, and remember, the intended place for them to dissolve is about 1-2M HCl solution.

the stuff is now in water, so presumably, filter out solids.

then a strong base boil, which will take care of what the acid didn't take care of, again, 5M sorta strength, put nonpolar on top to keep the goods from goin away, and extracting into it at the same time.

then, activated carbon clean, should remove dyes and crap like that, and then dehydrate with anhydrous epsom salts.

I'm inclined to think that the way to get the goo outta ya face at this point is to do things to change the salt you make into something insoluble. pfed oxalate is unfortunately very soluble, as is sulphate and HCl. It would be worth doing some experiments to find a low solubility salt of pfed, my money is on citrate.

then back to freebase, nice and gently, base with sodium carbonate and boil under reflux (it's incredibly easy to make a ghetto reflux with a test tube, some epoxy resin, and a chunk of rubber or better, a rubber stopper, make all the residual nasties separate from the freebase, then cool it down, should get a layer of fb pfed on top, and finally, convert the solid to acid by heating gently in acidic water of known molarity and slowly add more solution until it reaches expected concentration at which point the solids dissolve.

For good measure, a final defat, and then evaporate and recrystallise in methanol/ipa and dry acetone.

i haven't really suggested anything new or groundbreaking here, except maybe the idea of busting the pills up in a high boiling nonpolar using microwaves, but i think that putting all of the techniques together should guarantee the best results, and the method described here avoids water until the point at which its use must commence, and by then most gak should have been washed out in either ketone or chlorinated hydrocarbon, the acid boil is a new idea, based on the discovery that soaps are often part of the ugly mix, which i don't think has been tried or suggested, but is known to cause some polymers to decompose too... and then a double a/b including a freebase cleanup, carbon and defat at the end, should theoretically cover just about every kind of junk you would theoretically encounter if you theoretically extracted hypothetickal pills of any imaginary kind...

p2e3r4f5e6c7t8 · Wed Jun 01, 2005 7:15 am

Iv been away for a while ever since THE HIVE & RHODIUMS Site went down, And i was wondering if anyone has tried this KOH method using Ethanol ?????.

But none the less NICE SITE, eehheemmm shane_warne

p2e3r4f5e6c7t8 · Mon Jun 27, 2005 11:26 am

tina_craig · Mon Jun 27, 2005 7:47 pm

Yes, IPA and KOH does freebase the PSE, however, there is a new method at Wetdreams that works much better by WhoMe than the KOH boil and is completely over the counter with higher yields.

hAzzBEEn · Tue Jun 28, 2005 10:11 pm

I agree with tina_craig.
Try the Straight to Bee III method.
I re-listed it here on synthetikal for easier viewing.

Here is the link:

Straight to Bee III – The Pickled P

All of VideoEditor's extractions are top notch.

Previous extractions by VideoEditor:

SWIM has used both the "Straight to Bee" and the "Straight to E" methods with success

p2e3r4f5e6c7t8 · Thu Jun 30, 2005 10:25 am

hAzzBEEn · Thu Jun 30, 2005 7:25 pm

It was just a suggestion of a known successful method. Many bee's at WD report success. SWIH's not sure if the KOH method gets all the gak out. If you try it, report the results.

The STBIII method doesn't seem very complicated:

Extract with Brine/Filter
Neutralize
Boil/Basify w/ Non-polar
Separate/Crystallize

KOH method:

Extract with IPA/Filter
Boil/Basify
Extract with Nonpolar
Separate/Crystallize

If doing the KOH method, couldn't one just add everything(pill mass, KOH, IPA, Non-polar), boil, and separate? Would IPA need to be anhydrous? It seems that using even 91% IPA leaves significant water to cause problems.

Do you have a link to the original method? Where can it be reviewed?

EDIT: I just noticed that the method is the original post of this thread. Stupid me. After reading, it seems equally as complicated. Has anyone seen this method used with success?

tina_craig · Thu Jun 30, 2005 10:29 pm

1. You need water for the hydrolysis.
2. All the gaak won't be removed unless you use Fester's modification or switc's modification.
3. Never tried running it all together at once. Beware of bumping.
4. Switc has performed more KOH boils than she has reductions, which is a lot, the STBIII is the easiest extraction method she has ever used, and one doesn't have to obtain KOH, which switc could only find online.
5. If done properly the yields are higher with STBIII. Switc mastered 70% with KOH boiling she hasn't gotten below 80% with STBIII.