Post reaction separation of meth & e.hcl

[jammin]

Swims 2nd LWR-reaction has started.
He has lab grade i2 and RP. Extracted from european e.hcl pills...

He read here that the uasually contain l-ephedrine.hcl, but that it
could be used as psuedo in a HI reaction to create meth.

So he extracted the ephedrine from the pills using boiling IPA, and no
tetratraps etc cause the pills are just 6g of mass for 3 g of meth and
are from pakistan. I seriously doubt that they have same gak there as in
the US...

Anyway, postextraction weight seemed to match my predictions.
Got between 80 - 95% yeilds, pretty good i thought.

So, off to make the LWR going.

Added 10ml dH20 and 4 g LG RP to a 250ml RB flask.
Added 12g LG I2.
Smelled the HI forming.
Now i fubled a little, so it took me about 50 sec - 1 min to get all
the e.hcl in before i could mount the condenser with big assed balloon on.

Swim read that there was supposed to be bubbles all over the reaction surface
during the reaction. He observed his own, saw no bubbles. Feared that all HI was gone. Yanked up heat, oilbath now reads 125-128C. Bubbles can be observed but not over the entire surface at all times, but it bubbles ok, so he recons thats normal.

Now he wonders..

He has seen posts here that if psuedo is dirty he will get nothing
And if HI conc. is less than 57% he will get nothing.

So he figures of course to recryst. but is there any way to separate unreacted e.hcl and meth.hcl? He figures that it will follow in any recryst or wash he does...



Also, having never seen or done meth, how will he know that is is in fact meth
and not just e.hcl? or 20% meth and e.hcl?




Swim just wants a clean product, any suggestions?




Thanks for your time!

[jackhole]

Swim read that there was supposed to be bubbles all over the reaction surface during the reaction. He observed his own, saw no bubbles. Feared that all HI was gone.

Plain old water will bubble too, ya know.  Geezmeister (in particular, there are obviously hundreds others) knows this shit excellent; learn from his posts.

Now he wonders..

That's when it gets dangerous.

Yanked up heat, oilbath now reads 125-128C. Bubbles can be observed but not over the entire surface at all times, but it bubbles ok, so he recons thats normal.

I reckon yer reckoning is right I reckon.  Crank that oil bath temp up about 10-20 C more, becasue there's typically around a 50 C lower temperature difference of the contents in the flask as is the temperature of the oil bath.

He has seen posts here that if psuedo is dirty he will get nothing And if HI conc. is less than 57% he will get nothing.

Where? That's bullshit; the amount and type of inactive(s) present with the (pseudo)ephedrine in the reaction has the potential to destroy your yield.  In regards to the concentration of the hydrogen iodide, it's a 50% and lower concentrations where the reduction will slow to a halt, not 57%.  57% is a pretty fuming liquid anyway, just like conc. HCl.

[xaja]

...you've just rearranged your whole house for the forth time, reorganised the garage, washed the car, and you're considering asking the neighbours if they want their garage tidied while you're at it.  

And after a while you get to know if there's unreacted E present from the taste if you burn some in a glass pipe. This is something that comes with experience, can't think of any other way to tell really without NMR and other lab techniques. SWIM just used to throw some in the pipe, hit it with the flame, and inhale baby... You get to know the taste of success pretty well, as well as the taste of failure...

[jammin]

Yea, but what about separation?
Can anyone enlighten a bee fumbling in the dark?

[geezmeister]

I doubt that the HI produced in such wet conditions while you added the E, fit the condenser, and affixed a balloon was enough to cause problems. You saw no bubbles in the flaks because you didn't get it hot enough to make it bubble. You will see bubbles as the flask contents approach 100C. At 100C they will probably cover the entire surface of the reaction fluid. I run this type of reaction just below that, at a temperature where the bubbles cover about half the surface. The times I have measured this, the temperature has been in the 95-97C range. I normally establish the temperature by visual observation of the bubbling early on in the reaction. The temperature can safely vary up or down from this point with good success. The temperature inside the flask will be cooler than the oil bath temperature, and the difference can vary with the flask and condenser used, the size of the reaction, where the flask is positioned in the oil, I suspect your oil bath is about thirty degrees hotter than the temperature inside the flask. As the oil bath heated to the 125 degree temp, the contents of the flask started bubbling. This is as it should be. Let it bubble merrily away for a day and a half or so.

Everything sounds fine so far.

When you open that flask up after letting it reflux a long time your nose will note a distinctive odor no one really can describe because it only smells like what it is-- meth.
Do the workup and try a little bit. If its meth you will know very quickly.

Meth will smoke with almost no taste. Both E and pseudoE will give the smoke a bitter aftertaste, one that lingers for a little while and is not a pleasant taste at all. Meth also has a distinct taste, but I doubt I could describe it clearly enough for you to distinguish between it and the precursor. Some think meth tastes so bad it gags them, but I almost like the way it tastes. I'm sure I have acquired the taste for it, however. I do not care for the taste of E at all, however, and I suspect you will not either.

[Prepuce]

SWIP may bee missing something here, but has anyone thought of trying a separation of the post rxn mix? After basing the post rxn mixture the honey liquid floats to the top, while SWIM believes the solid pfed/E will mostly be disolved in the solution. (Or does it disolve preferentially into the honey oil?) It shouldn't be too difficult to do a physical seperation. It would make it easier to pour the solution into a column first, so the top layer can be easily seen and drawn off with a pipet or dropper.

PP

[12cheman12]

if you think you have some E still in you reaction fluid... cook it longer! give it a full 48 hours to make sure everything has been reacted.

[Scottydog]

I believe "fudgemonkey" was an advocate of using tap water.

Post 76048 (missing)

(fudgemonkey: "get the phed out.. 100% OTC, 100% effective", Stimulants)

He advocated the use of chloroform as well. I'm sure its all still buried somewhere in TSE.  

Swim has yet to try it out.

[mr_pyrex]

Yes prepuce, I came to the same conclusion that you had...which was that meth in freebase form is an oil and psuedo in freebase form is a solid, so therefore it stands to reason that you should be able to just basify your compound in something such as a burrete and then drain off the basic fluid and then recover the oil which would be the upper layer.  But as I have found there are a few problems that one runs into when attempting this seemingly easy task...first is that the meth oil seems to like to stick to the surface of the burrete...so when you go to drain off the basic fluid, the meth oil coats the glass all the way down until the bottom...and it doesn't rinse off the sides readily.  Next I believe that psuedo to some degree will dissolve in the meth oil, because after very careful and precise separation of the oil, followed by cleaning of the oil and then reforming the meth...it was clear that there was still psuedo present.  One other thing that might be of interest to anyone who wants to continue along those lines...be aware that meth oil will hold a fair amount of  water in it...so you'll need to free the oil of this moisture before say gassing it...or you'll find yourself with a whole new set of problems to deal with.  I have heard some mention that a steam distillation of the post reaction mixture once basified would be another possibility, although I have yet to try it.  I have now decided to try along the lines of separating by way of recrystalization(sp?).  So far I have done separation of some different substances by using acetone and isopropyl alcohol....I just dissolved a fixed amount of the mixture in the smallest amount of hot isopropyl and then added acetone until it just clouded and then let it sit until there was some solid materials that fell out of solution and then filtered those solids out and then let the mixture drop more out of solution and repeated until I had 6 different piles of solids that separated.  The results weren't encouraging, but it seems that it can be done, it is just a matter of finding the right solvents and a workable procedure.  I'm still working on it, keep you updated.  Pyrex out of scientific data ;-)