Extraction for name brand

[8ball]

[8ball]

[Jade]

Slow down a little bit.  Why don't you try starting out with typing just "sudafed" and go from there?  The search engine is only as "useless" as the "user".

[Rhodium]

Have you read the FAQ at the top of the Stimulants Forum Page?

[geezmeister]

I suspect most of us spend less money on generics, which are also more readily available in my part of the universe than the name brand medicines. The name brand also encompasses a number of formulations. Look at the extraction technique threads, and match up the inactives. I tend to avoid the name brand medicines as a rule of thumb.

[8ball]

Jade......   Slow down

Remember what i'm using Jade, It's not heroin.

Rhodium & Geez.....  FAQ & Extraction tecniques.

Have done both of these, ingredients listed on the box are pseudoephedrine hydrochloride 60mg and lactose cannot find any patent number on the box only exp date and batch numbers, so i thought bugger it i'll ring thier consumer healthcare number, and the bird on the other end did'nt have a list of insipient ingredients she could give me. So if anybody has anything on these pills i would appreciate some input.
               Cheers 8ball

[LoW_JacK]

Look, you've got roughly 90g. of the pharmecutical industrys leading pseudoephedrine producers product in them boxes there. Now this is good (90g.), and fucked up (it's sudafed). Now if i had 50 boxes and didnt know how to recover workable feedstock, i'd take one or two boxes and attempt a methanol extraction followed by an acetone crash then maybe an A/B extraction to finish with.

Maybe you'll find that it works, or maybe sudafed has invested in making their product so impervious to clandestine chemists extraction techniques that those 50 boxes are worthless. I doubt their worthless though.

The company should be giving you the inactive ingredients when you call them. Did you ask for that or what?
INACTIVE INGREDIENTS <-(key word)
Use it!

If they have a no-disclosure policy tell them that you are allergic to certain chemicals frequently found in alot of OTC remedies and need to know if their product is gonna make you flop like a fish once ingested. They'll either stick to their guns, or give the info.

have fun and take it slow if forced to figure it out on your own. Slow!!!

[8ball]

Cheers Low_Jack,
                 I'm actually half way through a metho soak at the moment and was going to follow up with a/b extraction, i was'nt going to crash with acetone but may as well through that in as well, a little xtra time is'nt going to hurt.

[placebo]

Sudafed has not changed their composition in Australia for some time. Why don't you just look up the extraction procedures that other Aussies have pioneered years ago?

[8ball]

Placebo i've had a flick through most of the posts concerning sudo extractions and either i cannot source some of the products used or do not have equipment for some procedures and there was'nt any thing relating a great deal to Oz (more so for chem substitutes). I dare say it's probably right in front of me, but just can't see it. Maybe i need some sleep.

[8ball]

Part 1

With 10 boxes(30 per box) of name brand 60mg pseudoephedrine hydrochloride whole tablets in a 600ml plastic bottle was added methylated spirits till full and shaken for 3 or 4 seconds while tablets dissolved, then left to settle for 1 1/2hrs then filtered through 3 coffee filters into clean beaker. Plastic bottle was again filled with metho again, but only to 2/3 full this time and filtered then once more to 1/2 full leaving for 20 - 30mins after a quick shake each time. With all filtered metho in one beaker still a little murky it was again filtered through 3 more clean filters coming through crystal clear then poured into a pyrex dish and evaporated until it started to thicken, maybe 125ml in pyrex dish.
At this stage i was getting a little lazy so instead of a/b extraction i decided to do Geez's pseudo precipitation technique using a microwave. So to 125ml of pseudo laden metho which had a slight yellow tinge to it was added approx 800ml of xylene, then zapped for 30seconds at a time until metho had completly evaporated and pseudo had formed itself in bottom of 1 litre pyrex jug. Fuckin like magic, totally awesome.So after a little jig in the kitchen with a grin like a cheshire cat saying to the missus "who's ya daddy" i proceeded to filter xylene through 1 coffee filter collecting just like Geez mentions pearlescant crystals.These were left to drain for 1/2 hour while i got my pecker sucked, then spread out on a piece of A4 paper to dry a little quicker. Once completly dry, about 2hrs they were weighed and come in at 14.6gms of 18 available grams of pseudo, this being only one filter from xylene, i would guess that there was maybe a couple of grams of pseudo and other bits of shit floating in xylene that was quite yellow to look at which had passed through first filter. Cheers Geez, i think that thread was under rated as only a good idea mate. I think it's fucken outstanding.

[halfkast]

I wonder if the microwaves have any type of effect extending beyond a simple boil through on a hotplate?

[SHORTY]

When using methanol and xylene it definetly has a benefit over using a hotplate.  Since the alcohol is polar then it is the main target of the microwaves so instead of heating only the bottom of the beaker which then heats the alcohol, you go straight to the alcohol.  I have found that when using the microwave it is best to use thicker glass like visionware.  The thinner lab glass gets hot too quick and then also cools to quick which can cause the gaak to precipitate before you can get the pseudo out.  I also found that putting one or two small pieces of glass like a from a broken glass stirr about 1/2 inch long in the mix you won't have to worry about bumping which is what used to scare me about using the microwave.  Microwaves will superheat solutions really quick and if your not careful then half the solution ends up all over the inside of chamber.  Xylene will dissolve the paint and then you can have a really big mess.  Also if you have a turntable, put the container on the outer edge of the turntable so that it moves constantly rather than just turning in the same spot.

[8ball]

I would'nt have thought that putting something in the container(ie. glass) would make a difference since the alcohol is underneath the xylene and is brought to boil to evaporate it, the steam and fumes have to escape somehow and the only way is via the xylene, so you are going to get shit everywhere anyway with bubbles exploding on top of solutions. I just put one of them microwave covers over the top to stop splashing. The ones you put over your tucker to stop it from going all over the shop.

[geezmeister]

The "xylene clean" method works much better if you do not concentrate the alcohol/pseudo solution. Pour the alcohol/pseudo mix into the xylene and heat the mixture up. An unsaturated alcohol/pseudo mixture is more miscible in the xylene, which you want. You will find the pseudo that precipitates will be cleaner and you will have better yields compare to a saturated solution.

[SHORTY]

I would'nt have thought that putting something in the container(ie. glass) would make a difference since the alcohol is underneath the xylene and is brought to boil to evaporate it

Just because the alcohol is underneath the xylene doesn't mean it will not superheat, in fact under those conditions it makes it easier to.  If there is a piece of glass in there to create nucleation points then you will find that the alcohol will boil at a steady rate and will not splash out when it reaches the surface.  Therefore you don't need to cover it and don't have to worry about lossing any as well as less chance of damaging the microwave.  You can also keep the power on rather than doing it in spurts.

Rather than pouring through a filter i find it easier to decant the dirty xylene.  With a beaker this is not easy to do but with a visionware saucepan it works great and since the pan retains heat its possible to follow the decant with a acetone flash which after decanted will dry in a matter of minutes.

[8ball]

Part 2...

In a 500ml twin neck rbf with liebig condenser attached in one neck 15ml of hypo acid was added then flask was placed in sink of iced water while 15g of I2 was added in 3 5g portions, once last portion had disolved 14.6g pseudo was added and flask swirled to mix ingredients.Second neck was plugged and rbf wasleft for ten mins to get back to room temp then heat was added very slowly until a steady reflux was noticed in condenser which held steady for 2hrs and 20 mins. Heat was turned of and the air conditioner was turned on to cool contents of flask down to produce a thick layer of fat that was looking quite promising.
Once cooled condenser was detached and replaced with angled splash head and then condenser fitted to splash head and water cooling pipes attached to condenser. A 10ml syringe was then filled with a caustic solution which had been prepared several hrs earlier to room temp.Once syringe was fitted to thermometer inlet(no therm)approx 1/4 of a ml was injected creating a shitload of smoke and then left to dissapate, then another 1/4 of a ml and so on until solution started to reflux from top of splash head and then heat was turned on low slowly increasingto the point steam was condensing at which point ph was tested and still a little low so more caustic was added until levels were at 13 - 14 at which time honey started to flowand cooling water was turned on. Everything was left as is until solution had near evaporated when 5ml of dh20 was added to syringe along with another 3ml of caustic and injected into flask creating another constant flow of oil drops to flow this was done once more along with ph adjustment ,after another 10 mins it was all over.
Caustic waste water was collected from under the honey and then remaining waste and honey were collected together  the syringe was pointed down left to settle for a couple of mins and then remaining waste water was dispatched and oil sqirted into evap dish and ph'd to 7 left to dry where once dry and weighed crystals came in at 11.18gms. so it's time for the tax man and then time to rextalize in alky.
           me bee buzzin

[SHORTY]

I have always added dh20 then do an np wash then base with 50/50 Naoh solution.  Then steam distill, drain water add np to fb in sep funnel and wash with brine and dh20 then add fresh dh20 and finally add hcl till ph7 drain and evap.

So have i been doing all these extra steps for nothing?

[wareami]

I'm curious as well about the removal of hypo prior to basing?
Bare with me as Ibee has never performed the hypo route.
Wouldn't the Hypo react with the naoh as it does with RP?
I guess as it's all liquid, there is no way to sep off the hypo prior to work-up...correct?
Peace of the _REaction
Have FUN-Bee SAFE

[8ball]

Shorty.     No np wash.

If i am reading you correctly shorty, you are draining flask after first reaction and being heated(refluxed)for 2 or more hours, washing with np and returning to flask and continue with distillation.
Why...Don't get me wrong this is how i was taught, the only thing i have changed is i premix caustic so it can cool down and also let the fat form on solution.

[8ball]

I have never done rp route so i don't understand that end either. I suppose it does in a sense(react with hypo)because when it hits the formed fat not a great deal happens but once the naoh breaks through to liquid solution beneath you in a sense get a violent reaction with hypo creating mega smoke and rapid boiling for 3-4 seconds in turn starting the distillation process. When adding naoh to flask it is very critical not to squirt a large amount or i dare say it would not be hard to crack flask, creating all sorts of drama's. I was probably being generous saying 1/4 of a ml, it would probably be closer to 1/5 maybe even 1/6. When i first started a couple of years ago i probably blew the splash head and condenser out of flask as the naoh would gel in needle needing force to expel contents then all of a sudden she would let go.
Like the bumping, i suppose you get used to it.

[SHORTY]

Wareami, the Hypo synth is the same as the rp synth in the end except you don't have to filter out the rp.  Both contain a mixture of hypophosphorous, phosphorus and phosphoric acids in addition to the HI as well as other shit that i don't know about. 

So basically, if he was doing a rp synth, then he would filter out the rp without adding additional water and without washing with an np, add the base and without adding any additional dh20 other than what was in the base solution, distill the meth fb off the top of the solution and then after distilling it add acid to the meth fb.  So in other words, he skips the washing phase completely.

I have always thought that this was neceasary in order to remove impurties which can come over in the meth fb even when distilled.

8ball,
When the rxn is complete i add dh20  about 2 times the vol of solution.  This is transfered to my sep funnel and a little more dh20 is added to the rxn vessel and then added to the sep.  I then add tol or xyl to this and shake, allow to seperate and drain the bottom layer into my boiling flask, add base, steam distill with sep funnel as receiving vessel and drain the bottom layer and discard.  I then add tol and wash with brine and dh20, then acidify and evap.  With 10-15g rxn this all can bee completed within an hour quite easily.

[8ball]

Shortie, I have never heard of any one doing this wash before but that dosent mean anything, with you doing a wash with np after first reaction, you say it only takes an hour to finish. thats wicked man and you do more work, i have sat there for 3 hours before , mind you not very often, but i will also double distill if waste water comes through any thing but clean, this also was something i brought on upon myself because i fucked up once and had all this white snow like shit through oil and waste water, its the only time i have seen anything penetrate the oil itself, as far as other impurities i cant imagine there would be to many coming over in oil itself. i seem to think the water holds any crap available. maybe , maybe not.

[SHORTY]

What do you mean the first rxn?  There is only one rxn that i know of unless you are calling the steam distillation a rxn as well. 

The np wash is standard procedure and is often mentioned by Osmium as well as most other knowledgeable bees.  Im not a chemist and don't know what it is suppose to remove but i beleive it is necessary.

Yes it takes me less than an hour to do the workup via steam distillation.

[8ball]

What do you mean the first reaction? There is only one reaction i know of unless you are calling the steam distillation a reaction as well.
First reaction is when you add I2 to hypo in turn creating HI.
The second reaction(i dont think you would get this after washing)i consider to be when i add the caustic solution to fatty acids causing rapid boiling and beginning the steam distillation without heat from electric burner.Once the steam builds up at the beginning of condenser i turn on the heat. My definition of a reaction i guess is when a number of substances be it 1 - 2 - 3 of them are combined creating(i dont know the right word to say what i mean, but reaction)something.I suppose like if you throw dirty old motor oil in a puddle, you see a reaction or petrol into a fire. I cant sort of explain the two differences between the two methods because i have never seen it done any other way, i guess thats why you dont understand what i am trying to say when i say second reaction. I think i have confused the both of us more now.hehehe. i know i am.
Let me know if ive made it a little clearer for you. i dont think i am sure my self now. i am in the same boat as you mate, i'm not a chem either, but i think you might be a good 10 steps ahead of me when it comes down to the knowledge side of things. What do they say "you can teach a monkey to copy anything" I was shown how to do it twice from someone even dumber than me and then left to ponder on what were the critical stages by myself. The bloke that taught me is blown away by the quality of my product compared to his. I guess it could be the same for you and i meaning i might be blown away by the quality your producing, yours i guess would have to be cleaner.Give my method a go, see what you think.

[8ball]

Using 10 x boxes of the pills mentioned above i have soaked in methylated spirits then metho drained through 3 coffee filters, this was done two more times to pill mass giving approx 1 1/4 litres of metho containing pseudo and whatever else crap is in the pills. Because i was in and out all day i did not evaporate with any heat for saftey reasons in case i left house forgeting hotplate on, so i just turned fan on lowest speed just to help evaporation process along before adding xylene and precipitating in microwave. Now when i finally get back (approx 8hrs)metho has evaporated from 1 1/4 litre down to 1 1/2 cups (375ml) now this remaining metho has a transperant skin across the top which i am about to filter of as garbage, but under the skin is a lot of semi solid white cloudy substance. Now the question i am asking is in a cup and a half of metho saturated with pseudo and whatever followed through in first 3 filtering stages, if i was to filter this solution with out heat so i dont dissolve these substances back into solution would i be filtering majority of pseudo and leaving only the crap or will the pseudo stay with this garbage.so does anyone know at what temp pseudo starts to crystallise or solidify.

[newworldorder]

grab wally world's El Cheapo model room dehumidifier (~$40)
remove it from its box without destroying the box
find or make something that needs to be evaporated - place it in the box and push the box up against the front of the dehumidifier

works wonders on slow evap solvents - ie 100ml of MeOH vanishes in 10 min.

and a superb smell squelcher to boot

[Un_Chambered]

You didn't read the geez man's replies well enough bro.
You absolutely don't want to concentrate your MeOH/pseudo solution to saturation,or at all for that matter.
Just add some more MeOH till everything dissolves and toss that in ur xylene for evaporation.
This way you won't have those problems,let the xylene decide whats garbage and whats good,it knows its buiesness.
Peace,ChambeRed.

[8ball]

Geez's method seems to work better when you have a volume of xylene that is quite substantial compared to MeOH solution, i had 600ml approx of xylene left and there is nothing in town until my order gets here. If you read my thread i had 1 1/4 litre of MeOH so i had to reduce this amount down considerably.But the point i was actually getting at was if i cold filtered the MeOH solution at that time with the floaties present was i going to lose a considerable amount of pseudo or not. So maybe you should start at the beginning and read all threads mate not just the last couple.

[SHORTY]

Just filter it cold.  I used to put mine in the freezer for a few hours and then filter to remove any waxes and other gaaks that would precip.  With that amount of alcohol compared to expected pseudo then your pseudo is still dissolved.  Of course a very small amount will bee lost but not enough to make a noticeable difference.

[8ball]

Cheers Shorty thats all i needed to know.

[tomjuan]

The problem is that your pills probably have either hydroproxyl methylcellulose or povidone (or both). There are techniques for removing both, and if you search around you'll find them pretty easily. However, what I have found is that it doesn't matter *what* they put in the stuff, if you don't mind waiting around for a while.

Normally, problems arise during the base extraction. When you add NaOH to your aqueous solution of pill extract, and try to add some toluene to extract it, you wind up with a big, emulsified mess. But if you put it on a shelf for a day or two, it *will* eventually separate. And if you are careful, you can decant off *most* of the toluene without getting the gunk in your extract. So if you don't have the skills, equipment or chemicals to do it the way that is recommended in earlier threads, just substitute time. Your emulsion will eventually settle (for the most part), and although your extraction yields will be reduced you will get sufficiently clean pseudoephedrine.

You should be a little concerned, though. If you don't have the chemicals and equipment necessary to pull of a clean extraction, you might want to ask yourself if you have access to everything you need to pull of the subsequent reaction.

[acx01b]

http://www.vidal.fr/medicament/sudafed-15691.htm

[geezmeister]

macrogol 8000.

Aye, there's the rub...