Author Topic: Successful [Large] RXN  (Read 14301 times)

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jackhole

  • Guest
Successful [Large] RXN
« on: November 01, 2003, 09:12:00 PM »
A 12-liter flat-bottom flask was charged with 700g (3.47 mole) pseudoephedrine, 840g (3.31 mole) iodine, 250g (2.02 mole) red phosphorus and 700ml water, and was lightly refluxed in a heating mantle for about 40 hours.

At the 40-hour mark, the flask was removed from the heat source and quenched with an approximately equal volume of water (2L), and 138g red phosphorus was filtered out.  The filtrate was returned to the flask, whereupon the flask was further diluted with more water to recover the last of the red phosphorus clinging to the flask.

The reaction fluid was taken up three times in 2L toluene, each time the toluene and reaction fluid vigorously shaken and the toluene phase discarded.  A 25% NaOH solution was used to basify the reaction mixture to pH 12.8, and the freebase was pulled three times in 1.5L toluene.

Anhydrous hydrogen chloride gas was generated in a separate 2-neck flask by filling the flask 1/3 full with NaCl and adding just enough 37% hydrochloric acid to form a paste texture.  Concentrated sulfuric acid was added dropwise with a sep funnel extending into one neck, and the generated anhydrous hydrogen chloride gas was bubbled through glass tubing extending from the other neck into the freebase/toluene mixture to precipitate a total of 550g (3.69 mole, 78.6% yield) product, which upon filtering displayed a completely white powder.  The solvent was subjected to bubbling a total of three times, the fourth time failing to precipitate any further product.

A bioassy revealed that no recrystallization was necessary, but a recrystallization was performed for cosmetic appeal.  The recrystallization was done from 99% IPA over a period of about 1 day to afford mostly clear shards over an inch long, quarter inch wide, and several ml thick.  It should be mentioned that not all of the shards were of this size, but rather half, the other half being gradually smaller down to the last <1%, which failed to grow larger crystals.

Note: The red phosphorus and iodine used both were of lab grade quality, and the pseudoephedrine was extrated from an array of pills per VideoEditor's "Straight to E" extraction technique.  No solvent boils before extractions or recrystallizations after were performed to the pseudoephedrine.


Rhodium

  • Guest
Great lab procedure, but the numbers are very off
« Reply #1 on: November 02, 2003, 12:53:00 AM »
Something is fishy with this writeup, as you say you had a 95% recovery of phosphorus, while in reality half of it should be consumed for you to be able to achieve that yield.

Also, as red phosphorous has a negligible solubility in aqueous solutions, it doesn't make any sense that more of it would precipitate upon dilution of the post-reaction solution with water.

Other than that, the lab procedure is excellent, other than the use of a flat-bottomed flask in a heating mantle.

When using solvent amounts like this, it is important to recycle it by washing it with brine (a concentrated table salt solution) and then distill it for reuse, collecting the fraction boiling within 2°C of 110°C, discarding the cloudy forerun and the impurity-laden residue.

callen

  • Guest
...and then bake at 400*.
« Reply #2 on: November 02, 2003, 01:54:00 AM »
Would you please state the temperature that you cooked at. I'm a little confused by the wide ranges of temps that I've read in various posts.Some say 150*c. for P-P Rxns, 180-190*F. for long, wet refluxes...or up to 110-120-to 125*c.Which is the way to go?


jackhole

  • Guest
Typo corrected - that 238g RP was 138g
« Reply #3 on: November 02, 2003, 02:04:00 AM »
And more water was added to the flask to recover some remaining red phosphorus which just happened to be stuck to the bottom of the flask.

Speaking of the flask: it was round, but with a flat bottom - not a volumetric/Erlenmeyer flask, if that's what you were thinking, but not a round-bottom fask.

The temperature of this reaction was actually never measured.  Heat was employed to create and maintain slight bubbling of the flask contents.  In reactions performed where the temperature was measured, 100-110 C was the required temperature for slight bubbling.  As this reaction had identical behavioral properties to all others (except for the size of it), it was assumed that the temperature of this reaction was 100-110 C.

The original write-up was corrected.


geezmeister

  • Guest
great meth
« Reply #4 on: November 02, 2003, 03:27:00 AM »
Sounds to me like you have a nice pile of very good methamphetamine. Good ratios, temps, times, enough water. You should have primo meth there.  :)

Now if we could just get some shorter-time cooks to try this a time or two, and see how significant a difference there can be with the additional water and time, at the lower temp and without the fuming and smoking.... but for some reason they just won't give it a try... like I didn't... for years.  :-[

Only took one long wet reflux for me to come around.  ;D


SHORTY

  • Guest
If timed right ....
« Reply #5 on: November 02, 2003, 04:31:00 AM »
I agree with geez.  For the impatient bees such as myself just start the next rxn before you run out of your personal stash and then you won't have to rush it.  For those worried about getting caught, if done properly, this can rxn is rather easy to run unnoticed even in a small apartment.


wareami

  • Guest
It's awe in the timing
« Reply #6 on: November 02, 2003, 04:58:00 AM »
I agree with shorty. Ibee was trying to come up with an extraction stategy for bulk extraction that would utilize similar thinking.
If one were to stockpile and get a headstart with just an extraction team, the cook could bee able to pump out stash regularly on time. The trick is in giving the extraction team the headstart!

I think jackhole's name should bee "jackpot". ;D  He sure hit it and I'm with Geez on his assumption!!! ;)


jackhole

  • Guest
No justification for a quickie of this size of RXN
« Reply #7 on: November 02, 2003, 07:05:00 AM »
There is no justification for rushing a reaction and "forcing" it to complete hot, when you're dealing with hundreds of grams :)   Or maybe there is justification, if you're attempting become the epitomy of 'pitiful' ;D


Osmium

  • Guest
> A 12-liter flat-bottom flask was charged...
« Reply #8 on: November 02, 2003, 01:57:00 PM »
> A 12-liter flat-bottom flask was charged with 700g (3.47
> mole) pseudoephedrine, 840g (3.31 mole) iodine, 250g (2.02
> mole) red phosphorus and 700ml water, and was lightly
> refluxed in a heating mantle for about 40 hours.


Why don't you give any more details about how the ingredients were added to the flask? In that order written above?

Did you encounter any problems during workup?


wareami

  • Guest
Good Question!!!
« Reply #9 on: November 02, 2003, 04:15:00 PM »
Osmium touched on a point that I was wondering as well!
How did the work-up GO?
Usually if there were any probs with gaak, they would manifest themselves in the final work-up if they weren't rid of on the front side!
Ibee could only fantasize about a rxn of that magnitude and he likes jackholes style concerning patience and mindset!
For ghettobees staying within the heat constraints, a 2liter winejug would suffice I would think. Just split the rxn in two and run them separately.
Ibee learned that Ideaology from jacked ;D
He also wouldn't consider anything but mixing in the order E and I2, dh2o, then RP....but that's just him!
Peace of the reaction

Have FUN-Bee SAFE



jackhole

  • Guest
Osmium & wareami...
« Reply #10 on: November 02, 2003, 05:47:00 PM »
This is the order in which the precursors were added:

1. Pseudoephedrine
2. Iodine
3. Water
4. Red Phosphorus

No details (or order) was given about how these were added to the flask because it is this bee's experience that the same outcome would have resulted, regardless of the order in which they were added.  As long as the iodine and red phosphorus aren't added in together, the addition order should be irrelevant to the reaction, work-up, and final product.  This wasn't mentioned because most bees should be aware of this, having read such info elsewhere or from personal experience!  :)

The only "problem" during this particular work-up was formation of a very small interface between the freebase and the reaction fluid during basing.  It must have been at most 1cm thick.  That was the only "problem" - like it was stated in my first post - a high yield was achieved, and the final product was indeed high-quality and bright white, without any further purification required.


Rhodium

  • Guest
Recrystallization is always required
« Reply #11 on: November 02, 2003, 08:16:00 PM »
Recrystallization is always required (unless you distill) when working up methamphetamine synthesized by any HI variation to remove any unreacted precursors, as well as the very toxic iodo-ephedrines and aziridines invariably formed as byproducts in the reaction. As they too are amines and form white hydrochloride salts, they will carry through an A/B, as well as being visually indistinguishable from pure methamphetamine.

wareami

  • Guest
Now cums the mass debate...
« Reply #12 on: November 02, 2003, 10:05:00 PM »
I beg to differ here rhodium but since I'm no chemist or have the ability or experience to precisely do a professional analysis, maybe I should just shut-UP!
But this is Ware here, so y'all don't get off the hook that easily! :)
Based on experience, I say that most of those impurities are taken UP and cooked off with the long wet reflux.
It's the very last selling point I have in my bag`o`treats as a salesbee! 8)
Ibee's done both the fasthot and dry plus numerous longwet refluxes and the difference in end product is like day and night ware impurities are concerned. The methods of analysis only consist of sight and bioassay.
While as you say these impurities cannot be detected with the naked eye for the reasons stated(all amines), their presence can be detected upon consuming said product.
In addition, the final work-up carries some visual clues as well concerning impurity types and amounts.
I do agree that good lab technique and protocol dictate that distilling or rextalling is required...
But I'll let you have the last word on whether my reasoning and experience carries any weight or validity regarding your admonitions to rextalize if not distilling.

Mind you, I'm not challenging your expertise in this area.
Just trying to understand better to improve the end result.

Generally with product that contains consistant amounts of impurities as a result of the reduction method, upon rextalling, the yield lost should be equivalent to those impurities. Correct?
What if after the longwet reflux and rextalling that this yield loss was very minimal.
Would the rextalling still bee a neccessary step?
Thanx Chief!


Peace of the reaction

Have FUN-Bee SAFE



jackhole

  • Guest
Yield loss is less than total impurities present..
« Reply #13 on: November 02, 2003, 10:16:00 PM »
I know this was directed towards Rhodium, but I'd just like to comment on a few things:

Impurities will remain even after several recrystallizations; if a recrystallization or several recrystallizations were guaranteed to remove all impurities, then virtually all recrystallized meth would posess the same psychoactive effect.

Recrystallization is required to compete visually with the current product flooding the streets nowadays, which happen to be huge, beautiful, crystal clear shards.  While the street product likely contains over 50% dimethylsulfonyl methane, it has been preferred time and time again over a purer product that is a powder.  Recrystallization affords a product that looks nearly identical to the huge shards, but with twice the potency, and only THEN is it preferred over the "glass" that is flooding the streets today.


WizardX

  • Guest
This Order.
« Reply #14 on: November 03, 2003, 03:59:00 AM »
I would do it in this order.

1. Water
2. Iodine
3. Red Phosphorus
Make your HI first, then...
4. Pseudoephedrine

Rhodium

  • Guest
Rxtal all Meth for the sake of your health
« Reply #15 on: November 03, 2003, 12:03:00 PM »
Based on experience, I say that most of those impurities are taken UP and cooked off with the long wet reflux.

Correct, in theory 100% of those byproducts will in time be reduced to meth, but without analyical equipment you do not know for sure if that has happened in each and every reaction you perform. There are also those minor freak byproducts (dimers for example) which cannot be reduced to meth still in the mixture.

While as you say these impurities cannot be detected with the naked eye for the reasons stated(all amines), their presence can be detected upon consuming said product.

I think that they can show toxicity at lower levels than is detectable by bioassaying. I bet you cannot feel any difference between pure meth and meth containing <1% aziridines/iodoephedrines, but even at those small concentrations they will be able to alkylate both DNA and other vital biomolecules in your body, leading to increased cancer risk and general deterioration of mucous membranes.

Generally with product that contains consistant amounts of impurities as a result of the reduction method, upon rextalling, the yield lost should be equivalent to those impurities. Correct?

Yes, if the recrystallization was performed with an optimal amount of solvent.

What if after the longwet reflux and rextalling that this yield loss was very minimal.
Would the rextalling still bee a neccessary step?


Not for the subjective experience of the product, but I believe that the time spent on recrystallization is well worth the lowered risk for cancer and other health-related problems.

geezmeister

  • Guest
note on reflux crystals
« Reply #16 on: November 03, 2003, 05:59:00 PM »
My experience recrystallizing meth produced in a long wet reflux is that the loss in weight is minimal compared to the push-pull product, and the crystals form much more quickly, all other things being the same. There appears to be less marked of an improvement in quality with the refluxed product, but there is a noticeable improvement.

Tweakers around here would rather have the raw powder, and complain the crystals do not give as "good" a rush or as "good" a buzz as the powder. While my opinion of "good" differs from theirs, the fact that they note the difference between the two suggests recrystallziation is still beneficial.


wareami

  • Guest
You may see me tonite with an illegal smile
« Reply #17 on: November 03, 2003, 10:31:00 PM »
It don't cost very much,
But it lasts a long while!

Thank You Rhodium and Geez:
My main concern was health related and both replys answered my questions and then some!
Ibee's end result is see through crystal clear.
Appearance WAS his guide prior to reading this!
He always wondered if further refinement would help minimize the health risks since he's never been able to associate a marked difference in quality through bioassay after rextalling compared to not rextalling.

Wizardx: Thank you as well because you reminded me of what Ballz and Orgy had been telling the Kidz all along!
Next romp in the mudpuddle they will incorporate that mixing sequence.
Peace of the reaction

Have FUN-Bee SAFE



Organikum

  • Guest
thats a way to do it
« Reply #18 on: November 04, 2003, 05:10:00 PM »
Hi made first - long refluxed 36 hours, already POPEYE told this being the biker receipt.

Another way to do this is to start with no water, RP, I, Pfed. PI3 is much stronger in halogenation action as HI, but this is a hot hot thingie - Jacked is best to tell. Of course if some GAA is used from start it is not so hot, H3PO4 works also. Later some water - depends on how dry was dry.... LOL
This pathway got fucked up at the HIVE as ppl added water from start. You cannot dance on both parties the same time baby.....

Nobody ever spoke of anhydrous.
You cannot say a reaction is bogus which is done a thousand times every day all over the world.


But actually the long wet reflux is the way to go. Add some GAA or H3PO4 and you will need much less RP/I.

And cut back on the iodine! thats actually whats killing yields and making byproducts! Oxidative cleavage of ephedrine by iodine is a usual way of determination of ephedrine content in plant extractions. All free iodine is bad. It is a catalyst - damned!
btw. it was was Osmipum who said that he thinks an oxidator like I2 in this reduction cannot be right.....

3 time molar iodine - the catalyst. The post is fraud anyways....
boasting, posting, boasting......


are you all glad to see me back?
yes?
smile
ORG


Rhodium

  • Guest
XS I2?
« Reply #19 on: November 04, 2003, 06:47:00 PM »
this is a hot hot thingie

And gives a not not pure product, consisting of large amounts of unreduced iodoephedrine/azridines.

Oxidative cleavage of ephedrine by iodine is a usual way of determination of ephedrine content in plant extractions. All free iodine is bad.

Can you provide us with references? I have only seen HIO4 being used for such cleavage. It sounds very interesting, and is a great argument for adding any (pseudo)ephedrine last of all, after all the iodine has been reduced to HI by the RP/H3PO3/H3PO2.