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Phlux's Quick Mescaline Hcl Recrystallization tek. Options
 
futura
#21 Posted : 7/19/2010 8:22:07 AM

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OK so now Im even more confused!!!

Lets see if I have this straight...

Dissolve Mesc HCL in a little room temp water

Add Ice Cold Acetone

Swirl around till solids precipitate out.

Decant and evap water/acetone mix

Repeat once again if desired to purify further

Re-x with MEK to remove non-mesc Alkaloids

Discard solids as they contain only trace amounts of Mesc HCL as well as other non desireable alkaloids


Is this Correct??

Thanks...

futura
 

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w0mbat
#22 Posted : 7/25/2010 4:17:45 AM

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futura wrote:
OK so now Im even more confused!!!

Lets see if I have this straight...

Dissolve Mesc HCL in a little room temp water

Add Ice Cold Acetone

Swirl around till solids precipitate out.

Decant and evap water/acetone mix

Repeat once again if desired to purify further

Re-x with MEK to remove non-mesc Alkaloids

Discard solids as they contain only trace amounts of Mesc HCL as well as other non desireable alkaloids


Is this Correct??

Thanks...

futura


This does not make sense... dissolve mescaline in a solvent mixture (water + acetone), then evaporate it. You'll wind up with exactly what you started with. Sorry if I'm misunderstanding something :/

EDIT: aahh ok. thx soulfood
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soulfood
#23 Posted : 7/25/2010 4:20:23 AM

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All you have to do is read the OP, then you see what happens when the acetone is added, allowing these non mescaline precipitates to be filtered out.
 
kemist
#24 Posted : 7/26/2010 6:54:36 AM

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ILPT think what would happened if one swap acetone for IPA.
As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 
Touche Guevara
#25 Posted : 7/26/2010 12:52:34 PM
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Has anyone come up with a hypothesis as to the composition of these precipitates?
 
Phlux-
#26 Posted : 1/4/2011 1:46:23 PM

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just did this again on 10g slightly colored mesc and was blown away by the results - seriously a viable tek imho
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Simplistic Randamonium
#27 Posted : 1/9/2011 3:04:07 AM

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will this work for acitates?
how van i convert my acitates to hcl?
if u made it this far you are a champ, and although we may never meet you are also my friend.
S.R.
 
DiMiTriX
#28 Posted : 1/9/2011 8:42:44 AM

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just put the stechiometrichally right quantity of hcl into
Tz'is aná
 
cker
#29 Posted : 1/16/2011 7:25:35 PM

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Forgive me but this thread is confusing and runs counter to what SWIM observed. The Wiki says Mesc*HCl is soluble in H2O and insoluble in Acetone. Doesn't this mean that the 1st small amount of H2O will dissolve all alks and then the Acetone will 'bomb' the insoluble Mesc*HCl out of solution? In that case, the Mesc*HCl will be the precipitate and stay behind while the alternative alks will be decanted off? If this is all correct, perhaps the tek could be added to the Wiki? If not, could someone explain why the Mesc*HCl stays In the Acetone even though it is insoluble?

Edit: I just re-read Burnt's analysis post. It answers lots of questions except Burnt didn't use a small amount of H2O to put the Mesc into solution prior to washing. I think that's a nice feature of this tek since it insures 'all' of the Mesc is washed. Does a small amount of H2O change the solubility of Mesc*HCl? I wouldn't think so, but idk. What would be very bad is for someone to read this tek and throw away (say) the decanted solid because it isn't Mesc(or visa versa) and thus waste the goods.

Simplistic- Mesc*Acetate is soluble in Acetone, H2O and IPA but insoluble in MEK. The WIKI says:

Mesc*Acetate Isolation: when mescaline acetate is extracted from San Pedro, Achuma, or Peruvian torch, it can be isolated from the other alkaloids by washing it in cold MEK (use 10 ml per gram of alkaloids, and wash 2-3 times). The non-mescaline alkaloids dissolve in the MEK, while the mescaline acetate does not. Mescaline acetate can be recrystallized in MEK by boiling the MEK and then freezing it overnight.



 
antichode
#30 Posted : 1/17/2011 6:57:55 PM

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cker wrote:
could someone explain why the Mesc*HCl stays In the Acetone even though it is insoluble?


Someone correct me if Im wrong, but in very simple terms..... You are changing the polarity of acetone with the addition of water, just enough so that the mescaline remains in the water/acetone but not enough for other alkaloids which are present hence why they 'crash out'. These alkaloids, whatever they are, seem to have a tan color and mild smell.

It does work rather well


 
mattritt
#31 Posted : 1/20/2011 6:44:01 PM

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Looks SOOOO good!! Wish I had some mesc HCl to play with!! Razz
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Mitakuye Oyasin
#32 Posted : 2/6/2011 8:38:27 AM

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Interesting tek. What was the amount you started with and what did you end up with? Thanks.
Let us declare nature to be legitimate. All plants should be declared legal, and all animals for that matter. The notion of illegal plants and animals is obnoxious and ridiculous.
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All my posts are hypothetical and for educational/entertainment purposes, and are not an endorsement of said activities. SWIM (a fictional character based on other people) either obtained a license for said activity, did said activity where it is legal to do so, or as in most cases the activity is completely fictional.
 
rOm
#33 Posted : 2/6/2011 1:40:14 PM

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Phlux- you're the best crystal photographer I know here ! Always a pleasure to see your pics !
Smell like tea n,n spirit !

Toke the toke, and walk the walk !
 
biopsylo
#34 Posted : 2/13/2011 11:41:56 PM

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ok,

so 500mg of acetate goo was dissolved in 10% hcl, then bombed with acetone.

fractions were separated and evapped. the procedure didn't produce the results that were hoped for, so all was scraped up and mixed back together. = sticky amber residue.

dry acetone was used to wash this goo 3 times, followed by a dry ipa wash.
this left some pale tanish powder in the dish+lint after solvents were pulled off. acetone was now dark amber.

the tanish powder (+ lint) was dried. this was dissolved in very small amount of water- approx 10ml. to this was added approx 50ml acetone. shaken. the lint settled out fast, and all was looking like the tek describes....... BUT then.... large white flakes start rapidly forming and falling out of solution. the acetone very cloudy, not really yellow.

let sit for a few hours, and the acetone has gone clear with a slight yellow tint with a pile of not powder, not crystal clumpy flakes almost white at the bottom in the acetone.

two fractions will soon be separated, but what is in each? what has been done here that is different? or is it?

 
moyshekapoyre
#35 Posted : 3/12/2011 5:43:03 AM
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I also got the results that biopsylo got, I think. What could we have done wrong?

I used 10g of dark mesc. Dissolved in some water then filled the jar with acetone just as described. Let precip fall out. Evapped liquid portion. Result is a sticky amber mess that I have no idea what to do with.

Another question is, why is it sticky? Does it now contain acetone? What else could explain the change in consistency? It has been thoroughly dehydrated... I really wish it were not sticky, as it makes it extremely hard to dissolve now...
 
futura
#36 Posted : 3/12/2011 8:28:32 AM

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Did you guys read the title of the post??

This works well for Mesc HCL...Not Acetate!!!!

For Acetate do the Ice Cold Anhydrous MEK washes...
 
Virola78
#37 Posted : 3/12/2011 10:22:16 AM

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according to my memory (its been awhile since i read those threads about mesc extractions)

method --> to clean crude:

99% MEK recrystalization --> mesc-HCl or mesc-acetate
99% acetone & 99% IPA wash --> mesc-HCl
99% MEK wash --> mesc-acetate
acetone bomb --> mesc-HCl

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I know that you believe you understand what you think I said, but I'm not sure you realize that what you heard is not what I meant.
 
Carrierwave
#38 Posted : 8/7/2013 6:30:43 AM

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Sooooooooooooo........... this tek, couple points to make here.

The tek reads "the clear solution above is filtered off and and evaporated to yeild."
Does this mean the liquid is evaporated? Or the remaining precipitate is evaporated?
And what does "The part that was washed off still contains a bit of mescaline" refer to, which part?

Tell you what happened when someone tried this: The mesc HCL dissolved in water, then "copious" amounts of -10 C acetone was added. Mesc HCL fell out of solution and was fluffy white. Now according to folks like soulfood and antichode the opposite is expected to occur: mesc HCL stays in solution while impurities fall out. Quite frankly that makes about as much sense as oil dissolving salt and water dissolving some non-polar thing. I'll explain why at the bottom.

Also the second post from OP says "The liquid portion evapped," and it shows some pictures, and so the first post must have meant to evaporate the precipitate; Right?

*southern accent* I do declare this thread a confusing conundrum. Only conclusion I can come to that makes everyone's opinions happy and validated is that depending on the ratio of acetone:water you either get a precipitate of mesc hcl or of junk.

Here's what I think the point of this tek is, and how I conceptualized it prior to being informed about the results.

~~~

Theory time:

Mescaline HCL extract has inherent impurities due to inaccurate titration which exhibit the color brown, these impurities are understood to be anything other than Mescaline HCL. In San Pedro they are 3,4-dimethoxyphenethylamine, 4-hydroxy-3-methoxyphenethylamine, 3-hydroxy-4,5-dimethoxyphenethylamine, 4-hydroxy-3,5-dimethoxyphenethylamine, anhalonidine, anhalinine, hordenine, tyramine, and 3-methoxytyramine. Now when performing acetone washes of Mescaline HCL crude extract it is best to crush the mescaline into as fine a powder as possible. This is to increase surface area of the extract in order to dissolve as much of the impurities as possible. However when mescaline HCL forms, since it is crystalline, it will trap impurities in its structure, and it is very difficult to entirely grind the powder into an ultra fine dust. Because of this limitation, acetone washes often leave the extract remaining some shade of brown, they do not completely dissolve the impurities. The impurities cannot be dissolved in acetone if they are trapped in the structure of the insoluble (in acetone) mescaline HCL? However, to sidestep this problem we can dissolve the mescaline HCL in water. When molecules dissolve their either separate into individual atoms, or into individual molecules. Mescaline HCL breaks apart into molecules, which increases their surface as close to 100% of maximum as anyone would care. This frees the impurities allowing them to actually come into contact with the acetone and dissolve. This step completely bypasses all grinding and crushing and far more effective. The acetone/water mixture would then need to be removed from the Mescaline HCL precipitate and the process repeated a couple of times to remove all the non-precipitated Mescaline HCL still floating, but not dissolved, in the acetone solution.

Forum Chemists, am I super fucking wrong?

The only way this cat can imagine the mescaline HCL dissolving in the solution is if it were 80%+ of water and only a small portion of acetone.
 
Kyle109
#39 Posted : 8/7/2013 9:56:35 AM

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beautiful thanks for the info il be doing some hcl soon
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dg
#40 Posted : 8/8/2013 2:51:03 AM
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Carrierwave wrote:

The only way this cat can imagine the mescaline HCL dissolving in the solution is if it were 80%+ of water and only a small portion of acetone.


no- acetone with a couple tiny drops of water will dissolve a surprising amount of mescaline
 
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