Mescaline Sulfate

DrugPhreak · Working Bee

SWIDP is about to dream of a mescaline extraction again and is out of EtOH. Is mescaline sulfate sparingly soluble in IPA also?

If it is more soluble... since IPA is insoluble in salt solutions this may not be too much of an issue. Or would that even apply here? Is it like only insoluble once the solution is completely salt saturated? I see that mescaline (like amphetamine) sulfate also contains two molecules of H2SO4, but it contains four molecules of water hydration/crystallization.

DrugPhreak · Working Bee

Nothing has been done yet, but when it comes to crystallization it seems like most teks are in error. They say to add 33% H2SO4 (aqueous) to the non-polar. Last time the chemist tried that a dark green slime formed at the bottom of the flask and the non-polar turned a pale green. This extraction was basically doomed for several reasons at the time though. This chemist thinks the amphetamine work-up should basically bee used with mescaline also. Mescaline freebase seems to bee more stable and boils at 353.5C (760mmHg) so I guess the chemist could just evaporate the non-polar in a beaker. It will form the carbonate if left in contact with the air too long though of course. Maybe they could do that with the amphetamine also and not have to bee bothered with distillation. Once the non-polar has evaporated they could dissolve it in anhydrous EtOH or ice cold 151/195 proof grain alcohol and then drip in alcoholic (EtOH) H2SO4 slowly in small amounts to precipitate the mescaline as the sulfate. Then it could bee purified with a little Norit and recrystallized from ice cold dH20, but if it was crystallized this way the majority of the product would bee mescaline anyway and probably rather pure. There was no miscibility data for IPA and toluene in the Merck Index so I did a few tests and I see they are miscible, but when water was added it formed three layers. WTF? Ethanol doesn’t do that. This chemist will have to wait a few days before they can do this extraction because their grain alcohol is currently being made. Also, any SWIY ever try gassing the non-polar?

IndoleAmine · Dreamreader Deluxe

Adding 33% H2SO4 to a nonpolar can't be right, since they are insoluble in each other! Better use alcoholic solvent (ACS grade MeOH) - you can always remove it with moderate vacuum if it proves to be wrong/too much...

And btw, mescaline sulfate contains one molecule H2SO4 and two molecules amine per molecule sulfate salt - not two molecules H2SO4 and 4 molecules H2O...

(maybe the reason for the previous failure was 4x excess H2SO4?

IPA and toluene are miscible in every proportion, unless you add so much H2O that the IPA is extracted with it. But never will you get three layers when you combine toluene, IPA and H2O (all clean!), and mix thoroughly. The IPA will always be divided between the aequous and nonpolar phase, but never form one separate layer - it is miscible with both.

You should try and mix and swirl them a bit...

I would try and recrystallize from IPA, if it doesn't dissolve with moderate heating you can add preheated d.H2O dropwise until it is dissolved, and if it doesn't precipitate, you can crash it out with ether or acetone...

Good luck!

DrugPhreak · Working Bee

Yep, I always thought that definitely wasn't the best way to go about things when precipitating the sulfate. Many teks do this though... there is one by someone named Nanook that obtained ~36gm of (crude) mescaline sulfate from 50 pounds of San Pedro. If anyone is going to go this route they should at least make the dH2O ice cold. Oh yeah, I should have looked at that at that closer... I see that it only has 2H2O being a dihydrate... etc. The previous extraction was done so poorly it could have been many things, but too much acid was probably added also. Tap water was added to the IPA and toluene (both lab grade) during that test so I guess it was some crap from the water that caused that issue/emulsion. Also, when Iso-HEET was used the IPA turned a milky white when water was added... God only knows what's in there though. SWIDP plans to work-up/crystallize like the amphetamine will be done. In the case of mescaline sulfate wouldn't ethanol be more suitable to make the alcoholic acid solution since it's soluble in methanol? When the Merck Index says "alcohol" for the solubility data of a substance I assume they are referring to ethanol? Is this the case or is it all the common alcohols?

MargaretThatcher · Mon May 16, 2005 6:19 pm

Nan's "The Nook" is back up.

loki · guinea pig

that whole business of proper acid/base ratios can be very confusing. the general method which results in proper acidification is to use something like 1/20 diluted acid and do little bits at a time until it comes out still acidic. if one makes a known molar concentration solution one can often know in advance approximately how much to expect to need to use. A titration strategy based on this could be set up so that one always adds half of what one expects in the remainder, so if you expect 0.1 M of alkaloids you add 0.05M worth of acid (or 0.025M for an acid with two acid thingies) and each subsequent titration use half as much liquid.

the thing about ratios, would that mean that citrate is 3:1 base:acid, since citric acid has three COOH groups? Tartaric acid has 2 as well, and if other tartrates are anything to go by it's probably quite low solubility as well. If one makes the phosphate, that's 3:1 acid:base too, cos phosphoric acid has three acid thingies too (moeities?).

with regard to crystallising, wouldn't it be possible to use another solvent to drive solubilities down, as is done with alcohols and acetone?

DrugPhreak · Working Bee

The alkaloid content of cacti varies greatly so it's nearly impossible to know what to expect without some type of high level equipment. Can anyone tell SWIDP for sure about the solubility of mescaline sulfate in IPA? They are just dying to do this extraction to see what they get and they have never tried mescaline before.

loki · guinea pig

mescaline sulphate is sparingly soluble in water.

why would you use something else?

mk-1 · Tue May 17, 2005 5:23 pm

why do u choose to make the sulphate over the hydrochloride? hydrochloric gas passed slowly thru a non polar layer containing ur amine base will yield in massive xtal formation. If u do it slowly enough u will not over acidify (which swim knows is a problem with acidifying amines).

DrugPhreak · Working Bee

Mescaline sulfate is sparingly soluble in cold water... the colder the better. It is soluble in hot water. SWIDP chooses to make the sulfate due to its easy purification from the other alkaloids via hot/ice cold dH2O.

IndoleAmine · Dreamreader Deluxe

mk-1: in the case of mescaline, the preferred salt is usually the sulfate, due to its ease of recrystallization. It also gives much nicer needles than the HCl... Wink

DrugPhreak: DON'T USE TAP WATER! Smile

(you know why)
Also I would maybe try and redistill your sovent before use. It doesn't sound like if you had pure stuff..

Anyway, as long as you don't use too much acid (and clean solvents), you can't make really big mistakes.
The salt once made is rather stable, you just have to make it come out of solution with any known method you can think of (cooling, decreasing solubility by ading other solvents, concentrating the mother liquor). If you use too much or the wrong solvent, thats no problem - you can always remove it with vac distillation and replace it with a better one (or with less of the same?..

Good luck!

DrugPhreak · Working Bee

Yep, SWIDP sure doesn't want to have a failure again like they had with the San Pedro extraction a few months back. Some high purity solvents are on the way. Wink

IndoleAmine · Dreamreader Deluxe

DrugPhreak · Working Bee

Thanks for the extra info! Wink

Who's PhugDreak though? Laughing

Also, do you know why the toluene turned green last time when H2SO4 was added to it? Confused

hest · Fri May 20, 2005 4:35 pm

I have made both salt's from alcohol (ethanole)
Adding HCl in ether to the alcohol yeald nice white powder
When making the sulphate I added app.20% sulfuric in ethanole to the ethanole solution and filtered off the produc. Then rex in wather. Nice xtal's
(And the best PEA iff you ask mee, but that a. diff history)