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Mescaline HCL Clean-up

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futura

futura

Rising Star
Ok, I have read all the teks...all 50 pages of 69 rons tek and all the posts of phlux's extraction and also his recrystalization teks and I am confused on one point of Mesc HCL clean-up...

To me as i read it 69 rons clean up of Mesc HCL and Phluxs Clean up of Mesc HCL give conflicting advice.

Phluxs tek calls for dissolving Mesc HCL in a little water then adding alot of cold Acetome and junk will precipitate out. The you filter out junk and evap acetone/water to yield cleaned-up mesc HCL. Then you do an MEK Wash to remove non mesc alkaloids.

So in short Phluxs tek says the mesc stays in the Acetone/water solution and the junk precipitates out...

69 rons tek says put mesc hcl in vial,add acetone and the mesc HCL sinks to bottom and most of the non-mesc stuff stays in the acetone, the you decant off acetone and wash mesc on bottom of vial with 99% IPA to further purify and remove non-mesc alkaloids...

Im confused because one tek(phluxs) says mes stays in acetone/water and the other tek (69 rons) says mesc HCL doesnt stay in the acetone but the junk does????

Both (the way I am reading it) cant be right can they???...so which is it?? or are they both right and Im missing something somewhere??

Can someone please help...dont want to lose my hard earned extraction to the wrong process...

thanks

futura
 
Im no chemist. And i havent done all possible cleanups as described here on the nexus or other forums... But i have followed 69rons tek and was left with some awesome washed mesc-HCl. Fairly pure from what i can say. From what i have read not all non-mesc alkaloids are washed away by acetone alone. So imo one must use (also, or at least) IPA to get rid of some nasty contaminations..

Maybe you want to check the posts by burnt about cleaning mesc-HCl, using acetone and IPA wash. He knows someone who tried in a lab. Someone who has equipment to test for purity. Here you have a small part of his posts about cleaning mesc-HCl:

From: san pedro alkaloids part 2 - Generic - Welcome to the DMT-Nexus

------------
Results:

Acetone rinse material (~95 mg): Had the same chemical profile as the crude mescaline except a major difference in ratios between compounds. Instead of mescaline being massively more abundant in the crude HCl mixture the acetone rinses contains an almost 2:3 ratio of 2,4DMPEA to mescaline. Also the other two alkaloids are more abundant relative to mescaline but they are minor compared to others.

IPA rinse material (~25mg): Also had the same chemical profile but mescaline was much more abundant again.

Cleaned mescaline HCl (700mg): Very pure. No impurities detected but probably with more concentrated injections some could be found. But this can risk overloading the instrument and is not necessary for this discussion.
-----------


:d
 
FUTURA they are 2 different approaches.

69ron`s swim taking DRY powdered crude mescaline HCL and dumping it into cold dry(anhydrous) acetone. With NO WATER presented mescaline HCL is not soluble in acetone so only contaminants(impurities) will be dissolved and after one repeated it 2-3 times he will end up with much purer mescaline.HCL


phlux`s swim`s approach is different and a bit harder to understand. He dissolving crude mescaline HCL in little water first. ( Everything apart airborn particles should dissolve in water as he obtained the crude hydrochloride by evaporating of HCL water. ). Then he added large ammount of acetone . While mescaline HCL still dissolved in solution (because acetone is not anhydrous and that little water is enough to keep mescaline HCL dissolved) polarity of this solution changed after adding acetone and some other alkaloids are no longer soluble .

ILPT cannot explain any closer what`s behind Phlux`s swim approach because phys/chem properties of the other alkaloids are largely unavailable.

he would like to know properties of DMPEA , 3-methoxytyramine , 3,5-dimethoxy-4-hydroxyphenylethylamine and 3,4-dimethoxy-5-hydroxyphenylethylamine. He knows little about tyramine m.p. is 155-163 C freebase has water solubility 1g/95 ml at 15 C whilst hydrochloride salt has water solubility >10 mg/ml
He also know that DMPEA has m.p. 12-15 C and it`s water soluble.

He would like to separate and purify non-mescaline alkaloids but there isn`t much info
 
kemist said:
FUTURA they are 2 different approaches.

69ron`s swim taking DRY powdered crude mescaline HCL and dumping it into cold dry(anhydrous) acetone. With NO WATER presented mescaline HCL is not soluble in acetone so only contaminants(impurities) will be dissolved and after one repeated it 2-3 times he will end up with much purer mescaline.HCL
Click to expand...

Ok I think I uunderstand...One more thing if you can please...

I didnt see a mention that the Acetone for 69 Rons tek had to be anhydrous...

So how do I go about making store bought acetone anhydrous???

I would assume I could use the same method to make 91% IPA anhydrous as well?? cause I cant find 99% IPA localy and rons tek called for a final wash with 99%IPA.
 
futura said:
kemist said:
FUTURA they are 2 different approaches.

69ron`s swim taking DRY powdered crude mescaline HCL and dumping it into cold dry(anhydrous) acetone. With NO WATER presented mescaline HCL is not soluble in acetone so only contaminants(impurities) will be dissolved and after one repeated it 2-3 times he will end up with much purer mescaline.HCL
Click to expand...

Ok I think I uunderstand...One more thing if you can please...

I didnt see a mention that the Acetone for 69 Rons tek had to be anhydrous...

So how do I go about making store bought acetone anhydrous???

I would assume I could use the same method to make 91% IPA anhydrous as well?? cause I cant find 99% IPA localy and rons tek called for a final wash with 99%IPA.
Click to expand...

Sure, sure, just tell swim to get driest solvent he can obtain and then use an anhydrous salt (MgSO4, CaCl2, etc.) to dry it out propery. Driest solvent , better yield = simples
Just to let you know preparing of some truly anhydrous solvents require of using vacuum distillation with elementar sodium or so !. :shock:

You rather stick with drying them with anhydrous salts !
 
[/quote]

Sure, sure, just tell swim to get driest solvent he can obtain and then use an anhydrous salt (MgSO4, CaCl2, etc.) to dry it out propery. Driest solvent , better yield = simples
[/quote]

Ok so I get some epsom salts..stick in oven for a few hours...mix in with acetone or IPA...shake well...let sit for awhile...then decant and filter...leaving me with anhydrous Acetone or IPA...

How much epsom salts to how much liquid should I use??

One more Chemistry question if you can help please...

I can only get 33-35% HCL(Muriatic Acid from Pool Store)). How do I dilute it to 10% ??

I remember some post that said 4 drops HCL in 10ML Water would give me 10% HCL is that correct???
 
No, no few hours, you weight your epsom put in in the oven and dry it until the weight is constant

How much of anhydrous epsom salt you need is hard to say because don`t know how much water is in your solvent. Add epsom until it`s not clumped and stucked on the bottom but it flowing as free powder in the solvent.

if you take 10 ml of your HCL and mix it with 35 ml of water you`ll get rougly 10 %
 
futura said:
..I can only get 33-35% HCL(Muriatic Acid from Pool Store)). How do I dilute it to 10% ??..
Click to expand...

If you need 10% HCl:


35% / 10% = 3.5 (dilution factor)

let's say you need 100ml of HCl 10%
then you take 100ml / 3.5 is about 28.57...

you will need about 28.5ml of HCl 35%, and then add water to make 100ml
now you have 100ml of 10% HCl


If you need 2% HCL:


35% / 2% = 17.5 (factor)

let's say you need 500ml of 2% HCl
then you take 500ml / 17.5 is about 28.57... ( 😉 )

you will need about 28.5ml of HCl 35%, and then add water to make 500ml
now you have 500ml of 2% HCl
 
why need a particular concentration of hcl?
just add it until the solution balances out ot ph 7, ie accurate titration...
cleaner product, and less work will be the result
 
benzyme said:
at pH 7, mescaline would not be 100% protonated, there would be 0.17% free base.
5.4 is the pH at which mescaline is completely salted.
Click to expand...

what ph does the ave salting tek take bring you to?
 
benzyme said:
at pH 7, mescaline would not be 100% protonated, there would be 0.17% free base.
5.4 is the pH at which mescaline is completely salted.
Click to expand...

irl, bringing the ph that low brings a lot of crude along for the ride
ever tried it?
 
benzyme said:
between 6 and 7.
it's generally a good idea to keep it lower.

a dirty bird did a crude sulfate extract where the pH was about 2.6 before evap.
he didn't re-x, but did a mp test on the sulfate salt. it melted at 180-185 C.
Click to expand...


can you point me to a salting tek that even gives or tests for ph range?
most saLT 3 times with fixed conc. of acid water--- they have no clue the ph/ and get cruddy product as result/needing repetitive cleanings
 
benzyme said:
between 6 and 7.
it's generally a good idea to keep it lower.

a dirty bird did a crude sulfate extract where the pH was about 2.6 before evap.
he didn't re-x, but did a mp test on the sulfate salt. it melted at 180-185 C.
Click to expand...

then ecxess acid would always be present, sulph doesn't dry out like hcl, so careful titration is needed
 
the salts actually completely dried out (by fan).

dg said:
irl, bringing the ph that low brings a lot of crude along for the ride
ever tried it?
Click to expand...

some dirty bird took the pH lower. the sulfate salts are off white, not much impurities present, and melt close to values listed in literature (~ 180-185 C vs. 183-186 C). mp range was determined using a Thomas-Hoover Unimelt, and is uncorrected.

the bird used what he's dubbed 'the marvin tek'. marvin is a molecular sketching and computational program; the pKa function gave those pH values, which is posted in another thread.

this is completely dry, after about 10 pulls from about 500 g dried SP powder. not recrystallized.
again, this melts close to lit. values, with about 5 degree range. est. ~85% pure
 

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sweet benz -- nice work,
in all my tests titrating below 6 made for more emulsions and dirtier polar solovent during salting.
see my dual solovent crystalization tek?
you are one step from crystaline needles :)
you'll be suprised how much crud will get left behind vs evap!!
 
dg said:
can you point me to a salting tek that even gives or tests for ph range?
most saLT 3 times with fixed conc. of acid water--- they have no clue the ph/ and get cruddy product as result/needing repetitive cleanings
Click to expand...

I think trout's tek (I believe it's still up on the nook archives) calls for salting w/ citric acid and measuring the pH to determine when to stop adding citric acid. My friend tried it for his first extraction ever, and could not pull it off. He now adds excess acid just for the sake of simplicity, but can see what you're talking about in terms of pulling extra crud...

Do you think you could take crude mescaline HCl that has been extracted with an excess of acid, freebase it again, and then salt it again carefully (not going below pH 7) and get a more pure product? Or will the crud still be there upon a second extraction?

benny - holy shit dude that bird is one lucky avian. Any idea what that all weighed? A character in a book I am writing is doing an extraction with an equivalent amount of torch.
 
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