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Bufotenine Extraction

Migrated topic.
Ditto that

SWIM would like d-limonene instead, but doesn't have the time to test it right now :(

SWIM would like to use d-limonene in all the techs requiring non-polar solvents. A mix of acetone and d-limonene is not that so bad. You can get food grade d-limonene and the acetone sold for doing your nails is USP grade (because it can get into cuts in your skin so it needs to be USP grade by law as far as I understand it).

I'm willing to bet that d-limonene will work in place of xylene. Even though it's more non-polar, it's chemical shape is very similar to xylene and it's boiling point is high enough that it would cause the bufotenine to melt, and that's the key to getting bufotenine soluble in xylene. If bufotenine is not melted, it's insoluble in xylene, only when it melts does it become soluble in it. I’ll bet the same is true for d-limonene, but the solubility is probably a little less. This test is high on SWIM's "things to do list" with his pure bufotenine when he has some free time.
 
Interesting results regarding FASA.

So swim did 3 acetone pulls, then boiled it down to about .75 liters. He added FASA drop wise, and this was too slow! Crystals kept coming out. Then swim just decided to pour FASA in. More and more precipitated.

Here's the strange part though. The solution turned ORANGE!!! as orange as Orange Juice. It still is that way. And swim is convinced that he can add even more FASA and it will keep precipitating (he added over 200ml of FASA). SWIM will just save the supernatant and see if more comes out.

SWIM will just wait a few more hours, decant the supernatant. Transfer the leftover crystals into a test tube, then filter the decanted liquid to salvage anything else.

E.C.
 
Update.

bufo-fumarate.jpg


SWIM's never seen a yield that high (not even from 250g of MHRB).

Given that a lot of it is particles that went through the T-shirt filter....and that it might be a little dirtier due to trace amounts of water....but after 4-5 washes or acetone, and then a MEK:Heptane wash....should be very pretty.

Update on the orange supernatant. After letting it sit for ~7 hours, swim noticed that it is in fact white precipitate giving it the orange translucency. He noticed that about about 1/8th of it settled, and saw very clear yellow-orange acetone. SWIM just poured off this supernatant, and will let it sit as it is, the white powder will eventually settle. SWIM will also try adding more FASA to it, since it most likely has more alkaloids in it. Either way, the massive amount of filthy crystals in the test tubes is very satisfying.

E.C.

EDIT: Now consolidated into 1 test tube. This stuff settles so quickly. SWIM has a feeling though that even after his acetone is near clear, the crystals will still be brown and disgusting. SWIM's praying for MEK:Heptane to do the trick.

Consolidated:

bufo-fumarate-1jar.jpg


Can't really tell from the picture, but the acetone is a piss-yellow color.
 
I think there is a lot of good info in this thread... 2 problems though

1. Boiling Xylene!!!
2. MEK, which is watched in many places

So if a tek using Limonene/acetone were to surface that would be awesome!

However, SWIM just got his cebil seeds in the mail and is willing to try the boiling Xylene method.

SWIM thinks the best way to do this is using a distilling device, and this will condense all the vapors to a liquid minimizing the smell (and conserving the solvent to some extent).

SWIM also has Pyrex crystallization dishes.

Only problem is image hosting, SWIM is really nervous about using imageshack and the like...
 
Another update: The salts have been washed and dried. This was strange, on swim's 4th acetone wash, the acetone got darker rather than cleaner. Oh well, swim thought it was originally nasty junk, but now that it's dried, it is a light tan color and the crystals are very visible. He will now freebase them once more.

Actually looks decently pure as it is, swim will test some before doing the MEK:Heptane wash.

Great TEK so far!

E.C.


EDIT: Here's the re-freebasing part...

re-freebase.jpg


SWIM added a little too much water (there's water drifting around in that dish), but it's not a big deal, swim will probably dry the whole mess in the morning anyway.

SWIM couldn't prevent those clumps from forming, and they are impossible to break up. SWIM has a huge feeling that the extract is much dirtier than he thought.

While cleaning that mess off of his hands, he rubbed his fingertips together (probably accelerating the reaction), and it turned into a BLACK GOO. It would not wash off his hands...soap and hot water. He had to use acetone to dissolve it off his hands.

After a few acetone pulls and evap, swim thinks the result will look something like that, and in that case, swim will definitely utilize a MEK:Heptane wash, which as Jorkest showed everyone in his fantastic pictures, leaves behind the black goo.
 
2 questions:

1.Does anyone know the difference of regular cebil and var. A. colubrina *Fat type* ?
Its half as expensive as regular a.colubrina.

2.Would this work to produce pure bufotenine crystals?

->Dry Seeds in the oven and grind them up
->Pour cold xylene over the seeds, stir, trash the xylene, dry the seeds
->Mix Seeds with Sodium Carbonate and water till it becomes a paste (ratio 2:1)
->Let it dry
->Dissolve the dried paste in Acetone,filter out the solids, keep the acetone
->Add citric acid saturated acetone to the acetone (or Fasa) ? to crash out bufo+toxins
->Mix bufo+toxins with sodium carbonate (2:1?) and water to form a paste
->let it dry
->Dissolve the paste with acetone and filter to remove sodium carbonate
->Evaporate the acetone to freebase bufotenine + Toxins
->Pour a mixture of MEK:Heptane (Acetone:Naptha, ratio yet to be determinated) over the gunk
->Filter and evaporate

----->Clear bufotenine Crystals

?
 
Not sure about the Fat Type..

That tek looks pretty solid (since it's exactly what swim just did!). Except swim would say that the Xylene step is unnecessary. It probably helps, but introducing Xylene is not worth it. Most the the fats and oils go away when swiy drops the bufo out with FASA (make sure to do a few acetone washes). Other than that, swiy could just do another MEK:Heptane wash.

SWIM just finished today! He only did 1 MEK:Heptane wash, he's sure that if he did another, it would be very clean...the current is clean enough for swim though.

Just a note: The product before the wash was awful...couldn't even scrape it up. Had to do the wash right in the pyrex dish. And then after evaporating the MEK:Heptane, swim thought he was stuck with oil again, it turns out the product was hard as a rock, very very crystalline.

His yield is: 676mg from 100g of seeds. This is a little low, but swim spilled a little a few times (stupid oversized funnels), and he did not do as many pulls as he could have. He also probably did not add enough FASA. SWIM can probably recover a lot more, but due to more mechanical errors, swim's yield from the recovery would be negligible.

Here's what it looks like (the crystals look darker than they are in this picture. In reality it's the color of caramel):

donebufo.jpg


Thanks for the TEK and help everyone. SWIM can't wait to try this out tonight and post back with a trip report.

E.C.
 
I wonder why it's so dark?

How did you do the MEK:heptane thing? Did you mix everything in the MEK:heptane, wait for it to settle down, and then pour out the solvent, leaving behind all the dark colored crap? Did you let the solvent evaporate on it’s own?

I'm exited to hear the trip report. I hope all the toxins are gone. It doesn’t look so clean.
 
Thanks ethnochemist!
Do you or anyone else know if citric acid saturated acetone works? IF so, any ration suggestions? Ok, I'll drop the xylene wash.

Concerning your extraction: Should these crystals look dark? I always thought them to be white.
 
Citric acid works better than fumaric acid. Fumaric acid works for DMT better than citric acid does because DMT citrate is somewhat soluble in acetone, but bufotenine citrate isn't. So for bufotenine, use citric acid because its both cheaper and more soluble in acetone.

The crystals should be clear or white, maybe with a slight yellow color.

They should look like this

resource.ashx


That's from the Name that crystal thread. There's more pictures there.

Those are bufotenine crystals that SWIM made using the MEK:heptane mix.

Prior to getting to that level of purity, SWIM did a standard A/B extraction that included several defats with DCM in the acid stage, and then he extracted with DCM in the base stage. After that he mixed the resulting goo in a 2:3 mix of MEK:heptane and then poured off the solvent leaving behind the dark colored goo and evaporated the solvent. He was amazed to see the crystals. I believe SWIM is the first person to use that solvent mix. SWIM was also amazed to find out that this process not only created the first bufotenine crystals SWIM ever saw, it also removed the toxins.

The crystals made from the xylene boil are more white than clear and are very small. They look like little dots of snow or something.
 
SWIM was wondering as far as extracting with ethanol, is that non-denaturated ethanol? Or is denaturated ethanol ok?

SWIM is liking the idea of a more natural extraction. SWIM is even bugged a bit from the fumes from heptane, even though he can't smell it through the mask, it still bugs him afterwards. He can't imagine what xylene must be like.
 
SWIM normally initially extracts with 91% IPA (don't use 99% by the way, it doesn't work as well). IPA is cheap and available at the pharmacy is USP grade with purified water as the only additive.

Ethanol or denatured ethanol should be just fine. As with using IPA, just make sure there's none left in the final product. Before using any new solvent always check that it evaporates cleanly. It is leaves behind a film, don’t use it.
 
polytrip said:
Are the other toxins besides unpleasant, harmfull in anyway?
Click to expand...

I don't know. I don't even know what alkaloids they are. It would be nice if someone could study them.

Here are the alkaloids known to be present in this plant. The toxins have higher water solubility than bufotenine. Bufotenine has an XLogP of 1.6. So the toxin or toxins are likely the compounds listed below with an XLogP lower than 1.6. That includes N-methyl-serotonin, Bufotenine N-oxide and Serotonin. The two beta-carbolines 2-methyl-6-methoxy-1,2,3,4-tetrahydro-9H-pyrido[3,4-b]indole and 1,2-dimethyl-6-methoxy-1,2,3,4-tetrahydro-9H-pyrido[3,4-b]indole have an unknown XLogP and could also be more water soluble than bufotenine and responsible for the toxic effect, but I just don’t know.

Code: 
XLogP Compound
?     2-methyl-6-methoxy-1,2,3,4-tetrahydro-9H-pyrido[3,4-b]indole (Unknown activity)
?     1,2-dimethyl-6-methoxy-1,2,3,4-tetrahydro-9H-pyrido[3,4-b]indole (Unknown activity)
1.0   Serotonin
1.3   Bufotenine N-oxide (Unknown activity)
1.4   N-methyl-serotonin (Unknown activity)
1.6   Bufotenine
1.7   DMT N-oxide
1.7   5-MeO-NMT (Unknown activity)
1.7   2-methyltryptoline (Unknown activity)
1.8   N-methyl-tryptamine (NMT) (Unknown activity)
1.9   5-MeO-DMT
2.0   DMT
 
Well, swim tried to smoke that stuff, it was unbelievably harsh...way harsher than DMT. Ususally with dmt, it's harsh at first, but the longer swiy holds it in, the easier it gets. For this stuff, the longer it stayed in (.5 seconds)...the harsher it got.

SWIM then did another wash on it (a lot of red/black sludge in it)....lost 2/3 of his yield and ended up with this...

donebufo2.jpg


It's considerably lighter, but then swim smoked that..and THAT was harsh too.

SWIM is now washing it again (now more of a caramel looking sludge), the nasty impurities sink to the bottom every time..a lot of them! The MEK:Heptane always takes on a slight yellowish tint. This wash right now is much clearer though, so hopefully the extract will be whiter, but the yield will suffer.

SWIM isn't sure if the harshness is from the crystals themselves or the impurities, probably the impurities considering how much in them (from these MEK:Heptane washes), but damn........very very painful to smoke...can't even hold it in. SWIM's yield will probably suffer once again, but as long as he gets AT LEAST ONE trip from this, he'll try again.

Sadly swim doesn't get many opportunities to do this extraction, he'll probably stick with snuff (which has worked for swim) or he'll try again with citric acid another time.

E.C.
 
SWIM found MEK in some hardware store, the official use had something to do with PVC pipes, cleaning maybe, dont know.


But SWIM still cant find pure heptane/hexane/naphtha. only a mixture that says 50-100% heavy naphtha, 2,5-10% 124trimetilbenzene and less than 2,5% xylene. How does that sound? Theoretically could one find a right ratio for purifying bufotenine with MEK and this mix SWIM finds?

how are the safety profiles for MEK and this trimetilbenzene (sp?)
 
endlessness said:
SWIM found MEK in some hardware store, the official use had something to do with PVC pipes, cleaning maybe, dont know.


But SWIM still cant find pure heptane/hexane/naphtha. only a mixture that says 50-100% heavy naphtha, 2,5-10% 124trimetilbenzene and less than 2,5% xylene. How does that sound? Theoretically could one find a right ratio for purifying bufotenine with MEK and this mix SWIM finds?

how are the safety profiles for MEK and this trimetilbenzene (sp?)
Click to expand...

MEK occurs in nature. It’s found in some trees, as well as small amounts in fruits and vegetables that humans eat, so humans have had MEK in their diet for thousands of years. It relatively safe in small amounts. I don’t know about the other stuff.

The solvents that humans have had in their diets for thousands of years include alcohol, acetone, d-limonene, MEK, and I’m sure a few others as well. All of these are safe to ingest in very small amounts because the human digestive system has evolved to cope with these solvents. They are present in small amounts in all sorts of foods we eat on a daily bases.
 
Hmmm, swim isn't exactly sure where to go with his extract right now...he's down to a pretty small yield so he'd like to make the best of it.

EDIT:

SWIM evaporated his MEK:Heptane once again, and it left crystals the color of a dmt extract with J. Spice. An orangish color.

SWIM thinks that more MEK:Heptane washes won't make em any whiter. Any other ways? (Other than Xylene boil, swim wants to avoid that at all costs).

SWIM did try to smoke this stuff, it was easier...but still unbearably harsh. SWIM is sure that near pure stuff is much easier to smoke.

Some effects noticed. Immediate effects: headache and bodyload, muscle soreness.........visual...sort of. It started off like when one stares at a bright too long, and when one closes his eyes, he sees the bright light lasting. SWIM saw that, and then it turned a very bright red..then curved as if it was the top of a candy cane, very vivid. But that went away in about a minute, and that was all.

Maybe a different ratio of MEK:Heptane? It always seems to take on a yellowish color.

E.C.
 
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