Washing mescaline

[69ron]

Very cool... Could probably get rid of the d-limonene taste by dissolving in water, separating out the remaining d-limonene, and then evapping the water again.

It’s not a show stopper though. It would taste good in juice as is. It’s just that the taste doesn’t go well with coffee, while the taste of mescaline acetate or mescaline HCl alone goes well with coffee (in small doses). The d-limonene flavor is just not something you want in coffee.

Has SWIY thought about saving some of the orange junk to test it's solubility properties? Would it be instructive to know if it were more less polar than mescaline acetate (i.e., as far as choosing which solvent to use to remove it from mescaline acetate)? The more we learn about the orange junk, the more ways we can find of eliminating it...

Yes, SWIM has a bunch of it for testing when he has spare time.

According to what SWIM found on PubChem, mescaline is the most polar of all the other alkaloids present. The orange junk seems less polar than mescaline acetate, or simply more soluble in solvents. There’s more to this than just polarity. Other forces are present.

I think the knowledge gathered from mescaline HCl and mescaline sulfate show that mescaline salts, in general, are more polar than the other compounds and not as soluble. For example, mescaline sulfate can be crystallized in ice cold water, but the other alkaloids cannot.

BTW, was the mescaline acetate your friend started out with from... San Pedro?

Yes, SWIM’s mescaline acetate in this case was from San Pedro.

San Pedro contains:

Anhalinine XLogP3-AA: 1.2
Anhalonidine XLogP3-AA: 1.3
3,4-dimethoxyphenethylamine XLogP3: 0.8
Hordenine XLogP3: 2.1
3-hydroxy-4,5-dimethoxyphenethylamine XLogP3: UNKNOWN
4-hydroxy-3,5-dimethoxyphenethylamine XLogP3: UNKNOWN
Mescaline XLogP3: 0.7
3-methoxytyramine XLogP3-AA: 0.9
Tyramine XLogP3: 1.1

Note that mescaline has the lowest XLogP meaning it’s the most polar of the alkaloids. Two have an unknown XLogP.

I think anhalonidine is the sedative in the orange junk. It has known sedative effects. Note that it’s documented that “Solns of anhalonidine acquire a reddish color on standing”. So that’s probably the cause of the orange color. Makes sense.

 

[w0mbat]

Doesn't the polarity of mescaline depend on what salt form it is in? Can get an idea of the polarity of the salt form by looking up the XlogP of the salt (e.g. fumaric acid)?

Am I correct in thinking that a salt that lowers the XlogP of mescaline more (makes it more hydrophillic & less soluble in nonpolar solvents) would be ideal?

Since mescaline is the most polar, but none of the alkaloids in the standard vinegar extract seem to dissolve in d-limonene, does that mean lower concentrations of IPA in d-limo (like, > 0% but < 11%) might dissolve them but leave the mescaline? (would this be what you meant by approximating the polarity of MEK w/ mixtures of IPA & limonene?)

And don't forget to update on how the xtal formation goes

 

[w0mbat]

Does anyone know if plastic syringes can be used to measure out d-limonene? SWIM's glass pipette broke and this is all he has right now to measure out precise ratios of d-limo : IPA

 

[kemist]

Does anyone know if plastic syringes can be used to measure out d-limonene? SWIM's glass pipette broke and this is all he has right now to measure out precise ratios of d-limo : IPA

ILPT using polypropylene PP turkey baster with no problems, only when messing around with DCM he using glass pipete as DCM dissolving his baster

 

[antichode]

Does anyone know if plastic syringes can be used to measure out d-limonene? SWIM's glass pipette broke and this is all he has right now to measure out precise ratios of d-limo : IPA

No they can't, the rubber stoppers soften and get stuck

 

[w0mbat]

This might be something of a tangent, but I just read that mescaline sulfate crystallizes out of cold water nicely. Does anyone know 1) if it is possible to get mescaline sulfate by mixing sulfuric acid with freebase mescaline-laden d-limonene, and 2) are there any ways to acquire food-grade sulfuric acid?

If FG sulfuric acid is easy to get, and it's easy to use it to salt mescaline out of d-limonene, this could make this whole discussion about washing mescaline acetate unnecessary - just imagine if pure crystals could be precipitated out of water...

Also, I seem to recall reading that mescaline sulfate might not be safe to use... can anyone speak to this or am I just making it up?

 

[69ron]

Yes, mescaline sulfate is easily crystallized from cold water, but sulfuric acid is very hard to get in food grade form.

Also, a lot of people have sulfate allergies, so it's not a good idea to use unless you know you can tolerate it well.

 

[w0mbat]

Hypothetical Experiment 1
Question: Can impure mescaline acetate be cleaned by washing with a solution of 89% d-limonene & 11% (nearly-anhydrous) IPA?

Materials: Food grade d-limonene; 97% IPA/3% water mixed with anhydrous magnesium sulfate (made by baking epsom salts) to produce ~99% IPA; impure mescaline acetate extracted from San Pedro. The starting amount of mescaline acetate was 299 mg, and it was dark red in color (using this color palate, it was approximately 71 R, 0 G, 0 B, or hex #470000).

Results:
The 299 mg impure mescaline acetate was washed with 6 mL of the 11% IPA solution. It was stirred with a glass rod in a glass container and large chunks of mescaline were broken up. The 11% IPA solution went from being clear to tinted yellow shortly after pouring it onto the mescaline acetate. The glass container was allowed to sit for about ~48 hours at room temperature to maximize probability that everything that could be dissolved was dissolved.

After about 2 days, the 11% IPA solution was poured off into a glass dish and placed in the freezer to see if anything would precipitate. As of now, nothing notable has. The washed mescaline acetate was dissolved in about 100 mL of distilled water, and this water was evaporated. After this, 0.188 g lighter-colored mescaline acetate was collected. Using this color palate, the washed mescaline acetate was about 255 R, 194 G, 102 B, or hex #FFC266. Bioassay has not been done. It was noted that the washed mescaline acetate was closer to being a free-flowing powder than the unwashed mescaline acetate, which was a little sticky.

Discussion:
-299 mg to 188 mg seems like a lot of loss! Perhaps the original sample was particularly high in non-mescaline alkaloids?
-Not sure what should be done with the leftover 11% IPA from which nothing seems to be recrystallizing. Maybe it should be left out to evap at room temperature for a while?
-What concentrations of IPA should be looked at in future hypothetical experiments? Would it be better to look at higher concentrations of IPA, or lower? The hypothetical goal is to get the highest purity mescaline acetate possible. Would higher concentrations of IPA be more likely to give a whiter, more pure final product, or would they just wash away more mescaline acetate (assuming any was washed away in this experiment at all)?


PS - ron, any updates on SWIY's recrystallization in the 11% IPA solution (the one that seemed to be producing 2 colors of crystal)?

 

[69ron]

After 2 days, the d-limonene:IPA wash stopped growing crystals and so SWIM decanted it, leaving behind the crystals. The wash was yellow, and obviously contained something in it that would not crystallize out.

The crystals that formed were separated into white and amber crystals and tested separately for oral activity.

The white was tested first. The effects were like that of pure mescaline. The texture was like that of freebase DMT.

The amber colored crystals were in fact mescaline that was just discolored with some impurities. The amber crystals were a little but sticky, but overall, the effects were that of clean mescaline.

The undesirable alkaloids that cause the “cactus fog” effect apparently stayed dissolved and never crystallized out.

It seems like the d-limonene:IPA wash dissolved way too much mescaline and it didn’t work that well in washing the mescaline. MEK works many times better. If the d-limonene:IPA mix was adjusted to be more polar, too much mescaline was washed away but a lot of colored impurities remained. It never really got very clean. If the mix was too non-polar, it didn’t dissolve much at all.


I think more things need to be tested.

The waxy texture of mescaline acetate, makes me believe it is very slightly melted at room temperature, very much like freebase DMT is, indicating it has a very low boiling point. This means it could likely be crystallized better in solvents that have a very low boiling point. This is a general rule. Freebase DMT can be crystallized in low boiling point solvents like heptane, but not high boiling point solvents d-limonene. Bufotenine with a high boiling point can be crystallized in d-limonene, but is hard to crystallize in low boiling point solvents.

With that in mind, think of what works for DMT, and try to apply a similar approach to mescaline acetate.

Freeze precipitation with a low boiling point solvent would likely be a very good technique for mescaline acetate. MEK has a low boiling point and mescaline acetate can be heated in MEK, will completely dissolve, and then on cooling, it precipitates out as very clean crystals. But not as clean as SWIM would like. Freezing precipitates out more than just the mescaline acetate.

My feeling is that ethyl acetate will work better than MEK. It’s almost the same as MEK but a little less polar.

 

[w0mbat]

Freeze precipitation with a low boiling point solvent would likely be a very good technique for mescaline acetate. MEK has a low boiling point and mescaline acetate can be heated in MEK, will completely dissolve, and then on cooling, it precipitates out as very clean crystals. But not as clean as SWIM would like. Freezing precipitates out more than just the mescaline acetate.

My feeling is that ethyl acetate will work better than MEK. It’s almost the same as MEK but a little less polar.

Has ethanol been considered for this purpose yet? Ethanol boiling point: 78.4; XlogP3-AA: -0.1; Ethyl acetate boiling point: 77 C; XlogP: 0.7.

Methinks it may be easier to just make mescaline HCl (possibly even using home-made HCl) and do freeze precip from 99% IPA than to acquire ethyl acetate, as it is a watched reagent and home synthesis seems quite difficult.

 

[w0mbat]

Mescaline HCl is somewhat soluable in 99% IPA at roomtemp (not very). It can actually be used (must be boiling) to re-crystalize Mescaline HCl to give crystals. It is used commonly in the literature to purify mescaline. Just let cool at room temp and let sit or place in freezer.

Has anyone ever tried this? I know ron mentioned washing with 99% IPA but this sounds different

 

[69ron]

Mescaline HCl is somewhat soluable in 99% IPA at roomtemp (not very). It can actually be used (must be boiling) to re-crystalize Mescaline HCl to give crystals. It is used commonly in the literature to purify mescaline. Just let cool at room temp and let sit or place in freezer.

Has anyone ever tried this? I know ron mentioned washing with 99% IPA but this sounds different

YES. SWIM has done it. It works very well. You need 99% IPA.

 

[kemist]

Ilpt done room temperature acetone wash on his impure mescaline hydrochloride which get rid of traces of limonene and some sedating alk. Now he has pinkish powder which has some other alkaloid in it apart mescaline. He would like to rex this impure powder from ipa to gain pure mescaline hcl but he also wanna retrieve the other alkaloid without evaporating his ipa. Any ideas how ? This alk. kicks in about 20 mins after ingestion. Is very speedy and causing bronchial dilatation. Do we know what it could be. Ilpt quiet like it and fancy to have it on it's own.

 

[69ron]

It would be nice to be able to separate them easily, that's for sure.

Notice that after the acetone washes, the mescaline still smells strong. Mescaline HCl is odorless. After a few 99% IPA washes, the order is gone and it's far more white. But from there, a few re-crystallizations in IPA are a good cleanup step and can get you really pure mescaline, or so I've been told. SWIM doesn't have the equipment to test the purity.

 

[burnt]

SWIM can try to theoretically find out what the 'other' alkaloid is hopefully tomorrow or day after. SWIM has some time for theoretical work, finally... This should clear up the confusion. SWIM also thinks it will help the community avoid ingesting unknown compounds.

San pedro is test subject.

So impure M HCl washed with acetone 2x and rexstallized with IPA. SWIM can analyze material before clean up and after clean up and what gets removed.

Do SWIMMERs suspect different alkaloids in acetone and 99% IPA washed or do SWIMMERS think its the same one? Either way SWIM will think about the whole mix.

Also is 99% IPA better then pure IPA?

Also ethylacetate might be fun to try?

 

[kemist]

Yeah mecsaline hydrochloride after acetone wash still smell.

Surely one more acetone wash will make it more whither but ILPT can`t be bothered. He somehow dislike smell of acetone and after working with it he can smell it in his room for another couple days. He used to work with it a lot in past and just dislike the smell

Majority of seddating alk was removed and that was his aim. Now week after the residue from evaporating acetone is not smelling of acetone anymore (finaly :d )
It`s blackish dark red sticky tar thingy which doesn`t look very good. ILPT knows taht his impure mescaline extracts with significant portion of this reddish stuff were far more visual first 2 hours then pure mescaline is. The visuals with open eye were sort of liquidy distortion very tryptamine like
But that were the acetate form not a hydrochloride

ILPT wanna clean this sticky tar up and turn it into acetate salt in one go. He was thinking to mix it with calcium hydroxide and dash of water then extract with limo and retrieve from limo with gar , then evaporate gar(good old tech, lol)

Any imputs? :roll:

 

[w0mbat]

Also is 99% IPA better then pure IPA?

AFAIK pure would be better; SWIMMERs just say 99% IPA to account for the fact that it's probably not completely pure IPA when you're making it from store-bought 97% IPA and anhydrous magnesium sulfate (afaik).

Also ethylacetate might be fun to try?

This SWIMMER would love to know how it works to clean up impure M acetate, but I suppose it's academic as ethyl acetate is beyond the reach of most home chemists.

 

[w0mbat]

ILPT wanna clean this sticky tar up and turn it into acetate salt in one go. He was thinking to mix it with calcium hydroxide and dash of water then extract with limo and retrieve from limo with gar , then evaporate gar(good old tech, lol)

Any imputs? :roll:

If I understand you kemist it sounds like the tar is already in the acetate form. If you just washed your impure M acetate with acetone, let the acetone dissolve stuff, decanted it, and then let it evaporate, the stuff it dissolved should still be in the acetate form.

 

[69ron]

SWIM can try to theoretically find out what the 'other' alkaloid is hopefully tomorrow or day after. SWIM has some time for theoretical work, finally... This should clear up the confusion. SWIM also thinks it will help the community avoid ingesting unknown compounds.

San pedro is test subject.

So impure M HCl washed with acetone 2x and rexstallized with IPA. SWIM can analyze material before clean up and after clean up and what gets removed.

That would be fantastic Burnt!

Do SWIMMERs suspect different alkaloids in acetone and 99% IPA washed or do SWIMMERS think its the same one? Either way SWIM will think about the whole mix.

SWIM has noticed two very distinct alkaloids other than mescaline. One is the sedating one which is easily washed away from mescaline acetate using either MEK or the d-limonene:IPA mix. It’s also easily washed from mescaline HCl using acetone. This is the one most people don’t like. It’s similar in effects to harmaline.

The other one seems to be a stimulant that lasts about 4-6 hours. When washing mescaline HCl with acetone, this stimulant washes away, but possibly some stays behind. It’s hard to judge the effects of it when the mescaline is in the mix because it feels similar to mescaline to SWIM. So SWIM is not sure, but thinks it’s the cause of the strong smell left behind after cleaning mescaline HCl with acetone. An IPA wash or re-crystallization gets rid of this smelly substance. It’s probably present in both the IPA wash and the acetone wash. SWIM never tried the IPA wash on it’s own though. He mixes it with the acetone wash and uses it like that.

Also is 99% IPA better then pure IPA?

I believe that pure IPA absorbs water from the air so I don’t think 100% IPA remains 100% IPA for long. SWIM can get 99% IPA at the local pharmacy. He’s not making it himself. I think there will be very little difference between the two because pure IPA is probably going to get wet from the air when you use it. That’s my understanding anyway.

Also ethylacetate might be fun to try?

This is something SWIM will try when he has free time. He has some ethyl acetate which he purchased for the purpose of crystallizing bufotenine (because of Jonathan Ott’s tech). But it’s actually a very poor solvent for use with bufotenine. Xylene is 100 times better because you can recrystallize freebase bufotenine in xylene by simply boiling it and letting it cool down to room temperature. It stinks really bad though.

 

[kemist]

SWIM has noticed two very distinct alkaloids other than mescaline. One is the sedating one which is easily washed from mescaline HCl using acetone. This is the one most people don’t like. It’s similar in effects to harmaline.

This could be the blackish dark red tar which ILPT has after evaporating acetone. He hasn`t tested it yet as it looked a bit impure to him, but he will tested it after he collect some more and does some clean up

The other one seems to be a stimulant that lasts about 4-6 hours. When washing mescaline HCl with acetone, this stimulant washes away, but possibly some stays behind.

ILPT disaqgree as after acetone wash his mescaline become very speedy and kicks in already in 20 mins
It seemed like the first blackish dark red tar sedating alkaloid counteract and killing the speedines of this other alkaloid. It also vary in consequent limonenene puls which explaining inconsistency in trips when whole mixture used to be taken

It’s hard to judge the effects of it when the mescaline is in the mix because it feels similar to mescaline to SWIM.

Ow c`mon ILPT can feel the difference very well.

IT`s STARTING TO BE NOTICEABLE IN 20-30 mins. There is no way mescaline hydrochloride would kick in so quick
It`s much more speedy and it also cause BRONCHODILATATION.
ILPT never heard of mescaline causing bronchodilatation

Effects of this speedy alkaloid subside probably 4-6 hours after ingestion but it`s hard to say as mescaline at this point running very strong. Definitelly can say that at 6 hours mark there is no more bronchodilation felt(so this alkaloid probably doesn`t last more then 6 hours)

ILPT wanna clean this sticky tar up and turn it into acetate salt in one go. He was thinking to mix it with calcium hydroxide and dash of water then extract with limo and retrieve from limo with gar , then evaporate gar(good old tech, lol)

Any imputs? :roll:

If I understand you kemist it sounds like the tar is already in the acetate form. If you just washed your impure M acetate with acetone, let the acetone dissolve stuff, decanted it, and then let it evaporate, the stuff it dissolved should still be in the acetate form.

NO NO NO NO NO NO :!:

ILPT turned his extracted impure reddish mescaline acetate into hydrochloride in order to clean it up with acetone and perhaps with IPA.

So his mescaline is in hydrochloride form and so is that blackish dark red tar.





THis is getting sooo exciting ILPT cannot wait to do ipa washes and then comparsion of different alkaloids.

He used impure extract many times, but inconsistency in trips realy pisses him off. Now he wan`t ingest impure stuff anymore. There is so much more in there and they easily could be more then 2 alks and mescalkine in his stuff. Wish he only has few days off