Bufotenine Extraction

[psychonaut]

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.

try evaporating only the MEK and let it recrystallize in the heptane.

 

[Ethnochemist]

They do recrystalize, but the crystals are so small that swim can't really pour off the heptane. (And there aren't that many crystals to begin with, so filtering wouldn't be a good idea). Maybe swim will try too pour off the heptane+crystals from the dish into a test tube so that the crystals can chill on the bottom, then he'll just siphon off the heptane.

But if the MEK has all evaporated, wouldn't the impurities already come out? The toxins aren't soluble in heptane anyway.

E.C.

 

[polytrip]

would letting the beans sit in cold water first, to get rid of the toxins, be a good method of reaching higher levels of purity, before doing an acetone tek?

 

[memo]

E.C. Sorry for the stupid question but just wanted to make sure that the crystals are in the freebase form and not the salt form. SWIM made the mistake of trying to smoke some of his fumerate salts and that didn't go over well at all. BTW SWIM has some Bufo in the black crystal stage after the second roll in sodium carbonate. He's planning on washing them with the MEK/Heptane solution.

 

[Ethnochemist]

@polytrip

Water probably wouldn't be a good idea since the alkaloids are in salt form and will probably dissolve in the water. Someone correct swim if he's wrong.

@memo

Yes, swim re-freebased his fumarate salts with sodium carbonate. Egh, the black/red stage is so disgusting, the first MEK/Heptane wash will take out so much of the impurities.

SWIM just wishes that the MEK/Heptane washes could get it cleaner, or that there was an easier way to smoke it.

E.C.

EDIT: Hmmm, maybe swim just needs to use less of the MEK:Heptane solution, he's been using 50ml of it for less than 200mg of extract, swim will try using just enough for his crystals (given the solubility 530mg bufo/100ml MEK:Heptane..thanks 69Ron). Maybe this will get them nice and clean.

 

[logos2012]

Try making a hooka that passes it through water first. SWIM did this for his DMT and it is much smoother. Can't even feel it in his lungs.

 

[Ethnochemist]

Try making a hooka that passes it through water first. SWIM did this for his DMT and it is much smoother. Can't even feel it in his lungs.

This probably works well for dmt, but swim isn't sure about how well it will work for bufotenine...since it's boiling point is so high, it might just condense in the water.

SWIM will probably make some enhanced leaf and try this anyway. Thanks.

E.C.

 

[69ron]

Because freebase bufotenine vaporizes at 320 C (608 F), the smoke is always a little harsh.

Keep in mind that freebase bufotenine is more pleasant if you don't take large hits all at once. It's better to space it out using small hits over a 5 minute time span. You’ll get a much better experience that way. It's not like DMT, where you quickly get tolerance to it so you need to smoke it all in one or two hits to get the most out of it.

 

[Ethnochemist]

Hmmm...swim actually kind of noticed that. When he vaped it, there was a large hit that he coughed up immediately...but then got a really tiny one afterwards that he could hold in..and that's what probably gave him the trip.

Any advice for taking small hits with a test tube pipe? Once it starts vaporizing, the vapor becomes really dense and swim can't even take a small hit.

Should swim load his dose up 2-5mg at a time (hopefully swim could do that in 5 min), or is there a way to get less dense smoke....maybe inhaling as soon as he sees the first tiny trace of smoke...before it gets too dense.

E.C.

 

[Ethnochemist]

Well, swim tried vaping his extract in small increments (as soon as he saw vapor he inhaled).

The first hit swim coughed up after 2 seconds....the other hits swim could hold in, but they were a little smaller. Vapor also stopped showing up as easily after the 2nd hit...no way swim smoked it all already.

The trip started with the tingling at about 3 min and a considerable body load. No real visuals...and swim felt this really weird sickness....it wasn't nausea, but his body felt bad...very strange.

It seems as if the bufo was in the first hit..and the rest of it crystalized somewhere else in the test tube, but the impurities made it to swim's lungs no problem.....since these effects seem like the effects of the toxins.


SWIM will try to wash this stuff more, but if that doesn't work...there's not much swim can do except find a way to hold in these hits. SWIM's used to high temp chemicals....like Salvinorin A...but that stuff never irritated swim's throat as bad as this stuff....even more than DMT!

E.C.

SWIM's guessing that the bufo was mostly in the

 

[urtica]

the original recipe calls for '1 part' calcium hydroxide... 1 part being 100grams? equal to the weight of the seeds??

 

[Ethnochemist]

Hey 69Ron....

Did swiy ever try this tek that swiy posted a while back?

SWIM wants to try de-fatting 100 grams of crushed seeds with 500 ml of pure MEK a few times until the MEK comes out clear, then freebasing the seeds in saturated sodium carbonate, and then extracting 3 times with 200 ml of a 40:60 mix of MEK to heptane (that’s a total of 600 ml, we only need 400 ml, so it’s a little excess just to be sure we get everything). Then boiling down to 50 ml and leaving to sit overnight. I think this could produce nearly pure crystals. SWIM will try it with his next batch of seeds.

SWIM has about an ounce of seeds left...and since this procedure is so simple (especially on a small scale)....swim might try it out. He'll adjust all the volumes, but this tek seems like it would work. So much less complicated too.

Just a note....what does swiy mean by "Saturated Sodium Carbonate"? Does swiy mean making a very concentrated solution of water and sodium carbonate....then doing a liquid-liquid extraction with MEK:Heptane? (SWIM might just use 10% ammonia then, and do liquid-liquid extraction) Or would it just be easier to do the wet-not-watery routine?

E.C.

 

[nux]

Just a note....what does swiy mean by "Saturated Sodium Carbonate"? Does swiy mean making a very concentrated solution of water and sodium carbonate....then doing a liquid-liquid extraction with MEK:Heptane? (SWIM might just use 10% ammonia then, and do liquid-liquid extraction) Or would it just be easier to do the wet-not-watery routine?

As far as i know, liquid-liquid extraction is not possible with MEK:Heptane because MEK and water are miscible. The freebased seeds must be dried before they are extracted with MEK:heptane.

 

[Ethnochemist]

Oh...well now swim knows.

Thanks nux!

Yeah in that case swim would just freebase normally with sodium carbonate. Seems like a solid TEK. One part swim doesn't like (nothing major) is evaporating the MEK off of the seeds before freebasing. Does MEK stick to it like Xylene (the xylene smell NEVER seems to go away!!!), or does it evaporate cleanly and quickly?

Or would it just be better to add a small amount of acetone to the seeds so that the MEK evaporates with it?

E.C.

 

[Exarp]

* Add 1 part pickling lime (calcium hydroxide) and mix in enough water to make it wet. NOTE: sodium carbonate works as a substitute for lime in all steps of this extraction tech.

* Evaporate the collected acetone to get nearly pure freebase bufotenine.

SWIM is going to extract some Yopo seeds using Ron69s Acetone Citrate Bufotenine Precipitation Tech (this seeds are from, now closed, Amazonhealing, so that means they are some 1 and half year old and probably not "true" Yopo).
SWIM almost get vertigo reading this whole tread :lol: . So informative and so...WOW!!!
SWIM can find n-heptane (it's used like thinner for nitro paints, smells very sweet). Acetone and Epsom salt isn't problem too.

So SWIM have 3 questions:

1. Sodium carbonate replaces calcium hydroxide in ALL stages?
2. Anyone found ratio for (eventual) acetone:heptane in practice?
and 3rd, to SWIM the most intriguing :
HOW much "nearly pure freebase bufotenine"?

SWIM made extraction that Norman suggested in the beginning of tread and ended up with a dark/amber goo that after a few days hardened and looked like a piece of plastic.
After evaporation of a small, (some 3 matches-head size) peace it looked like almost nothing is gone, but SWIM take a 3 tokes, none of them felt harsh, and some slight body load symptoms. This symptoms, compared to snorted seed/Na-bicarbonate mix, looks like fun:lol:
The visions vith eyes closed ware very interesting (dependent on light source). All bodily effects fade away in 5 minutes and replaced with nice "high".

When visions stopped, the nice high remains. Then SWIM smoked just a little, about a match-head size of pressed X-DMT (the yellow oil that left after SWIMs final DMT purifying, which was dissolved in 96% alcohol, and left for EtOH to evaporate leaving some sort of yellow christals which scratched have some brownish color).
SWIM didn't get some visuals (but there was some minor "moving" on ceiling), but felt very, very, veeeeery euphoric.
And emphatic; so much LOVE...
SWIM needed to immediately Skype his buddy to speak & laugh with him:d. This euphoric state lasted for another 30 minits, and after that just vanish, easy and slow as it started.

Anyway, SWIM is gone a little off-topic..sorry...

SWIM hopes that Citric acetone method will pull much cleaner product because SWIM thinks that toxins, beside that they produce unpleasent effect, they are ruining the "strength" and quality of Bufotenine trip.

 

[69ron]

Hey 69Ron....

Did swiy ever try this tek that swiy posted a while back?

SWIM wants to try de-fatting 100 grams of crushed seeds with 500 ml of pure MEK a few times until the MEK comes out clear, then freebasing the seeds in saturated sodium carbonate, and then extracting 3 times with 200 ml of a 40:60 mix of MEK to heptane (that’s a total of 600 ml, we only need 400 ml, so it’s a little excess just to be sure we get everything). Then boiling down to 50 ml and leaving to sit overnight. I think this could produce nearly pure crystals. SWIM will try it with his next batch of seeds.

SWIM has about an ounce of seeds left...and since this procedure is so simple (especially on a small scale)....swim might try it out. He'll adjust all the volumes, but this tek seems like it would work. So much less complicated too.

Just a note....what does swiy mean by "Saturated Sodium Carbonate"? Does swiy mean making a very concentrated solution of water and sodium carbonate....then doing a liquid-liquid extraction with MEK:Heptane? (SWIM might just use 10% ammonia then, and do liquid-liquid extraction) Or would it just be easier to do the wet-not-watery routine?

E.C.

No he never tried that. The last extraction SWIM did before that post yielded a ton of crystals. SWIM will probably not do another extraction for several months.

No liquid liquid extraction was intended, but it’s sort of similar. To saturate water with sodium carbonate you add 30 grams of sodium carbonate to 100 ml of water. You mix this saturated liquid with the seeds making a thick stew. Then you spread it thin and evaporate the water in an oven at about 170 F. Then extract with the MEK:heptane, or at least that was SWIM’s plan. He never tried it.

SWIM did something similar. He defatted the seeds with acetone, then freebased them with saturated sodium carbonate, dried it, and then extracted with acetone. It works pretty well.

SWIM still normally does an A/B extraction on them because you usually get cleaner results.

Just a note....what does swiy mean by "Saturated Sodium Carbonate"? Does swiy mean making a very concentrated solution of water and sodium carbonate....then doing a liquid-liquid extraction with MEK:Heptane? (SWIM might just use 10% ammonia then, and do liquid-liquid extraction) Or would it just be easier to do the wet-not-watery routine?

As far as i know, liquid-liquid extraction is not possible with MEK:Heptane because MEK and water are miscible. The freebased seeds must be dried before they are extracted with MEK:heptane.

MEK is more soluble in heptane than water. It’s only 27% soluble in water. You can use it for an A/B. Once the water contains 27% MEK, the rest of the MEK floats to the top of the water. I think if you add heptane, less than 27% of the MEK will go into the water, but I’m not sure about that. Also, I believe adding salt will make MEK less soluble in the water.

Oh...well now swim knows.

Thanks nux!

Yeah in that case swim would just freebase normally with sodium carbonate. Seems like a solid TEK. One part swim doesn't like (nothing major) is evaporating the MEK off of the seeds before freebasing. Does MEK stick to it like Xylene (the xylene smell NEVER seems to go away!!!), or does it evaporate cleanly and quickly?

Or would it just be better to add a small amount of acetone to the seeds so that the MEK evaporates with it?

E.C.

MEK evaporates really fast and cleanly if you spread the material out thin. It doesn’t leave any smell like nasty xylene does.

To give you an idea of how fast it evaporates, here are some evaporation rates of several solvents (Butyl acetate=1):

DMSO     0.026
Water    0.3
Xylene   0.6
Ethanol  1.4
IPA      1.7
Methanol 2.1
MEK      3.7
Heptane  4.3
Acetone  5.6

1. Sodium carbonate replaces calcium hydroxide in ALL stages?
2. Anyone found ratio for (eventual) acetone:heptane in practice?
and 3rd, to SWIM the most intriguing :
HOW much "nearly pure freebase bufotenine"?

If using sodium carbonate, yes replace calcium hydroxide in all stages.

SWIM wrote that tech a while back. I’d say about 80% pure. I depends on the seeds used. Some seeds have lots of toxins. You can tell by the results you get. If the results are dry, hard, and brittle, then it’s about 80% pure. If the results are sticky, probably 50-70% pure.

 

[Ethnochemist]

Thanks for the reply.

SWIM did something similar. He defatted the seeds with acetone, then freebased them with saturated sodium carbonate, dried it, and then extracted with acetone. It works pretty well.

Based on that experience, would swiy say that the results from that experiment would benefit from a MEK:Heptane purification? Or is it pure enough as it is?

SWIM was thinking that the MEK:Heptane extraction was pretty efficient in this sense, since the MEK:Heptane would just leave behind any extra toxins in the seeds from the start (after defatting and freebasing that is).

In other words, would doing the tek with MEK and MEK:Heptane make it unnecessary to do the defatting/extracting with acetone and then purification?


Could one technically defat with both acetone and MEK at the same time? or separately? would that be more efficient than just using one solvent?...or is one just better than the other?

E.C.

 

[69ron]

Thanks for the reply.

SWIM did something similar. He defatted the seeds with acetone, then freebased them with saturated sodium carbonate, dried it, and then extracted with acetone. It works pretty well.

Based on that experience, would swiy say that the results from that experiment would benefit from a MEK:Heptane purification? Or is it pure enough as it is?

It will make a big difference. Definitely do the MEK:Heptane purification.

SWIM was thinking that the MEK:Heptane extraction was pretty efficient in this sense, since the MEK:Heptane would just leave behind any extra toxins in the seeds from the start (after defatting and freebasing that is).

YES, it should.

In other words, would doing the tek with MEK and MEK:Heptane make it unnecessary to do the defatting/extracting with acetone and then purification?

YES.

Could one technically defat with both acetone and MEK at the same time? or separately? would that be more efficient than just using one solvent?...or is one just better than the other?

E.C.

It’s almost always better to defat with more than one solvent or solvent mix. For this case, since you’d be using a MEK:heptane solvent mix, It would be best to defat with the MEK:heptate solvent mix until nothing else comes out. Then for an even better defat, defat at least one time with MEK alone, and one time with heptane alone. There’s no need to use acetone. Acetone is very silimar to MEK in terms of what it pulls out.

 

[69ron]

A “defat” is really just an extraction where you’re trying to extract everything except the target alkaloid(s). We are commonly calling this a “defat”, but it is technically not a “defat”, it’s an “exclusive extraction” where we extract but exclude the target alkaloid(s) from the extraction. It’s more of a “cleaning” that an “defat”. This “exclusive extraction” extracts all sorts of things, not just fat and oil. The more of the non target alkaloids(s) that we extract during the “exclusive extraction”, the better the end product will be during the “inclusive extraction” were we do extract the alkaloid.

In this case, the target alkaloid is bufotenine. In it’s natural salt form in the seeds it’s insoluble in heptane, naphtha, MEK, acetone, DCM, xylene, and d-limonene. For the best possible defat, you would defat with a wide range of solvents in addition to the solvent or solvent mix used for the freebase extraction (the “inclusive extraction”).

Each solvent has some compounds it extracts better than other solvents. A “defat” is an extraction that excludes the target alkaloid(s). If you’re planning to extract freebase bufotenine with a 2:3 mix of MEK:heptane, you would get the cleanest results if you defat with MEK:heptane several times and then defat at least once with MEK, then heptane, then acetone, then DCM, then xylene, and then d-limonene, etc. The more solvents you use to “defat” the cleaner your extraction will be in the end. Most of your “defats” should use the solvent or solvent mix used for the final freebase extraction.

When doing the “inclusive extraction” or “freebase extraction” after you’ve “defatted” and then freebased the bufotenine, it’s best to use a solvent or solvent mix that best targets only the alkaloid(s) you want. It’s best to use a solvent that is not a wide range solvent. You want to extract just a very narrow band of things, as narrow as possible.

Heptane is a very poor solvent, it can only extract a small amount of target compounds. Many freebase alkaloids are very poorly soluble in heptane (mescaline, bufotenine, psilocin, “jungle spice”, etc.).

MEK is a wide range solvent, capable of extracting all sorts of things. Most freebase alkaloids are very soluble in MEK. By adding heptane to it, we are lowering the polarity and narrowing the range of compounds we can extract. The more heptane we add, the more non-polar the mix becomes.

There could exist another solvent or solvent mix that excludes the toxins and better targets the freebase bufotenine than the 2:3 MEK:heptane mix.

In general, non-polar solvents are more exclusive than polar ones. For example, ethanol is a very polar solvent, more so than acetone or MEK, and can extract pretty much every freebase alkaloid there is, and a bunch of fat, oils, and other junk as well, and all solvents are soluble in it from water to heptane. It can also usually extract many alkaloid salts that MEK or acetone can’t extract. It’s an extremely wide range solvent. The wide range most inclusive solvents include DMSO, IPA, ethanol, and methanol. The narrow range, more exclusive solvents include heptane, naphtha, xylene, and toluene. In the middle you have diethyl ether, chloroform, DCM, MEK, and acetone.

After freebasing, before doing the “inclusive extraction”, if you do another non-polar “exclusive extraction” with a non-polar solvent that the target alkaloid(s) is/are insoluble in, then your final product will be cleaner. For example, after freebasing, bufotenine is still insoluble in heptane. So you would extract with heptane. This would extract several non-bufotenine alkaloids making your final product that much cleaner. And then you would extract with the 2:3 mix of MEK:heptane. This would extract the bufotenine, but not the more polar toxic alkaloids.

So basically, for the best results, during the acid stage, do several “exclusive extractions” (“defats”) with a wide range of solvents. Then during the base stage, do several “exclusive extractions” that with solvents that don’t extract the target alkaloid, and then do an “inclusive extraction” that extracts the target alkaloid and little else.

Another thing that helps is pH. Bufotenine has a pKa of 9.67. So at pH 7.67, only 1% is freebased. So this is the best pH to “defat” at. So “defat” at pH 7.67, to remove non-bufotenine alkaloids that freebase at 7.67 (most of the toxins freebase at or below this pH) as well as removing fats, oils, and other junk. And then bring the pH up to 9.67 to extract freebase bufotenine. If you bring the pH up to 10.67 more junk is extracted along with the bufotenine. 8.67 would be the most selective pH for bufotenine but you’ll need to extract a lot more times.

This pH trick is commonly used for extracting mescaline from peyote which has a ton of different alkaloids in it. Mescaline has a pKa of 9.56, very close to bufotenine. If you defat the cactus at pH 7.56 (at that pH mescaline is only 1% freebased), you’ll remove a lot of non-mescaline alkaloids from the cactus as well as other junk. If you then adjust the pH to 8.56 (only 10% is freebased), and extract many times, you’ll extract mostly just mescaline, and leave behind other alkaloids with a higher pKa than mescaline.

 

[Ethnochemist]

69Ron.........you are so awesome! Excellent explanation! This is very very appreciated.

Quick question though. So say swim was extracting the MEK:Heptane mix..........and he did the "defats" with MEK:Heptane, then MEK, then Heptane until the solvents came out perfectly clear for EACH solvent...would an acetone, DCM, Xylene etc. "defat" really help? SWIM understands that it would get rid of the toxins that the others didn't pick up, but if swiy is extracting it with the very same solvent (MEK:Heptane), will it pick up toxins? How would the same solvent suddenly pick up toxins that were washed away before?

E.C.