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Pure DMT Fumarate from freebase DMT

Migrated topic.
No idea to be honest, I was also amazed that precipitation formed upon addition of fumarate saturated acetone, but still, this physical property of dmt fumarate can be possibly used to our advantage;)
 
Thanks Ronue

Hey, it's great to see more people taking an interest in salting. It's been bugging me for sometime now.. good work to have good people on the case 😉
 
Ronue said:
Upon drying the crystals off acetone they appeared fairly solid, however as time passed they turned gooey (presumably due to the absorption of ambient humidity). The goo was collected and dried at 37 C in the presence of silica beads to give crystalline dmt fumarate that could be easily scraped off the dish. The final product weighted ~130mg (good, this was expected for a starting material of 100mg dmt freebase).

This final product did not turn gooey again in the open air.
Click to expand...

Gooey indeed..

Do you think there could have been some water in the acetone?
And when you say dried in the presence of silica beads.. can you describe the procedure?
 
There shouldn't have been any water in the acetone. SWIM believe that it was ambient humidity that was absorbed on the crystals.

As for the silica gel, SWIM just used a simple desiccator with with a layer of silica beads to absorb the moisture from the crystals. The desiccator was placed in the 37 C oven just to speed up the process.

At least this verified that gooey crystals are the result of water. SWIM in a previous attempt tried to speed up the acetone evaporation by blowing air from his mouth on the crystals; Boy, the crystals ended up so wet that they assumed the viscosity of honey. They were ok however after they were forced-dried by silica gel,

SWIM thinks that a silica loaded desiccator is a good idea because the silica is a sink of humidity, both for the crystals and their immediate surroundings.
 
OK, SWIM determined that 1 ml of acetone can hold ~20mg of fumaric acid at room temperature, fairly neat since SWIM now makes dmt fumarate just by dissolving 66.666mg DMT per 1 ml of fumaric acid-saturated acetone and then evaporates it.

Notes to my previous post:

1)desiccator is not absolutely required for converting the dmt fumarate goo into solid dust; the process of drying the goo can take some time (~1 day) at room temperature and the end product is very nice and easy to handle.

2)upon determining the amount of fumaric acid acetone can hold, 10ml were evaporated and the fumaric acid was weighted. SWIM noted that condensation started forming on the thin layer of fumaric acid after the evaporation of acetone, converting fumaric acid to a goo. Given some time, it was completely dry and immune to further gooey-zation.

Now SWIM thinks that acetone will generally attract humidity when it evaporates; SWIU just have to give it some time for this little amount of water to evaporate when attempting to make dmt fumarate.
 
just a thought

methanol dissolves the freebase just as easily as the acetone, and it dissolve fumaric acid easier than the freebase. When neutralising one solution with the other, no precipitate is formed, but that doesn't matter if you're evaporating to recover. The benefit then is that you could perform easier pH testing on just the solution rather than a solution with precipitate present. Once neutralised or slightly acidic it can then be evaporated and the resultant dried to yield the fumaric salt. What you think?


Here's a quick question for you chem heads:
SWIM had a dream of dissolving 300mg of freebase in methanol. Then dissolving around 300mg of fumaric acid in methanol. The fumaric acid methanol was used to neutralise or slightly acidify the freebase in methanol solution. Once neutralised, two volumes of hot isopropyl acetate were added. Upon cooling, it was hoped that fine white crystals of dmt fumarate would precipitate, however unfortunately this was not the case. Nothing happened
The process came from: http://www.lycaeum.org/books/tihkal/07--2a-dmt.shtml

Any thoughts?
 
methanol dissolves the freebase just as easily as the acetone, and it dissolve fumaric acid easier than the freebase. When neutralising one solution with the other, no precipitate is formed, but that doesn't matter if you're evaporating to recover. The benefit then is that you could perform easier pH testing on just the solution rather than a solution with precipitate present. Once neutralised or slightly acidic it can then be evaporated and the resultant dried to yield the fumaric salt. What you think?
Click to expand...

SWIM thinks that it is absolutely fine, as long as one weighs fumarate and dmt accurately. That is to say that you can do it with methanol and evap, but any unused fumaric acid will be present in the final product. In addition, I do not know why you would like to perform pH testing.

SWIM likes the fumarate-saturated acetone because you cannot use too much of it; what SWIM did yesterday was to take 7ml of his fumarate-saturated acetone and dissolve 400mg of yellow xtals in it. Almost immediately beautiful precipitate formed which was collected and now it is drying.

SWIM also has a concern in the back of his head about solubility of dmt-fumarate in acetone. it looks as if it has zero solubility but SWIM will try to determine experimentally if any actually dissolves. SWIM's also got plans for further purifying dmt with this method, that is using acetone to clean up any oils and other impurities present in dmt fumarate. Possibly fumarate-saturated acetone can also be used for the same purpose since the already presence of fumarate may discourage the dissolution (if any!) of dmt-fumarate.
 
What i noticed was that for the small amount tested (150mg spice), the precipitate settled not much faster than it took for the acetone to evaporate. If you are forming the precipitate and then pouring off the solvent then acetone is clearly choice, but if you're evaporating to recover then i guess it shouldn't matter which solvent is used as long as both components are soluble in it. I like pH testing, it's interesting to see what's going on and have better knowledge that the reaction is complete rather than assuming it is based on numbers. I must agree though, the precipitate does look pretty darn good :d
As 69ron points out at the start, MEK could be used to purify

is is a coincidence that our two newest chem heads are both called Ron, kind of?

question for you Ronue, how many times do you recrystallise before proceeding salt?
 
hahaha, definitely a coincidence!

As for the spice used, it had been recrystallised only once, and it was not the whitest spice in the world. Rather yellowish I would say, I however reasoned that:

1) should the yellowishness come from dmt-N-oxide, then there is no reason why this shouldn't form a salt

2) should the yellowishness come from any lipid impurities then they would be washed off the after the dissolution of spice in the fumarate-saturated acetone. This is indeed what SWIM abserved; He dropped the spice in the solution, precipitate formed, precipitate sedimemted amd the acetone from above had a yellowish coloration while the sediment was much much whiter (but with a hint of yellow). This yellowish acetone could not form further sediment after addition of more fumarate-acetone.

So, for SWIM the most likely explanation for the yellowishness is possibly lipid impurities. But that shouldn't matter when salting is done via this fumarate-saturated acetone method.
 
This is a great site! So many people are very helpful here. It’s good to see so many other people doing tests!

SWIM loves this idea of using fumaric acid saturated acetone!

Are you sure the precipitate is DMT fumarate? Has SWIY tested it for activity?



Here are some interesting bits of information about fumaric acid (from A Dictionary of Chemistry and the Allied Branches of Other Sciences):

* fumarates are decomposed by hydrochloric acid, sulfuric acid, phosphoric acid, and nitric acid, producing salts of the latter and freeing the fumaric acid.
* fumaric acid decomposes acetates freeing up acetic acid and producing fumarates.
* "Many furmarates dissolve in water, but none in strong alcohol."

Is that last one true? None dissolve in strong alcohol? None?

Some more info from The Popular Encyclopedia:

* fumaric acid is precipitated from solutions by the addition of other acids.
* fumaric acid is very stable and cannot be oxidized.
* fumaric acid is not destroyed by nitric acid.

I think fumaric acid definitely has some unique characteristics that can be leveraged.
 
SWIM got interested in 69ron's post and did some test on the solubility of dmt fumarate in pure alcohols and acetone.

The fumarate salt he used was coming from yellowish dmt and had a yellowish colour itself. Please note this because there's a weird observation regarding the colour of SWIM's dmt fumarate.

Anyway, 5ml of methanol, ethanol, isopropanol or ecetone were saturated with SWIM's dmt fumarate, then the solvent siphoned off and evaporated. The residue was weighted. The results are:

Acetone : practically 0mg/ml (there was a very thin layer of residue left, impossible to scrape

IPA : ~1mg/ml. The residue was still too little to be weighted properly

Ethanol : ~5mg/ml

methanol: ~10mg/ml

Now, the colour of the fumarate salt collected from methanol and ethanol was fairly white, much much whiter than the starting yellowish fumarate that was dissolved in the beginning.

SWIM has no explanation about that....

SWIM also snortet 50mg of his dmt fumarate; Didn't burn and even though SWIM could feel it, it was not annoying. As for the experience, it only gave him a strong body load for ~1 hour. Should SWIM go for 100mg? 150mg?
 
Thanks for the solubility tests! THAT'S VERY USEFUL DATA!

I'm so glad someone has the time to do these tests!

Both DMT freebase and DMT citrate are soluble in acetone. But those tests show that DMT fumarate is insoluble in acetone. That’s quite interesting. That fact could be helpful in creating an acetone based tech that doesn’t require a non-polar solvent. Think about it. SWIM’s acetone citrate precipitation tech for Yopo could be adapted to Mimosa by substituting citric acid with fumaric acid. Hmmmm…very interesting.

I AM EXCITED!!!!!8)

Imagine this tech based on that info. Purely theoretical:

1 - Mix powder mimosa with 1 part calcium hydroxide.
2 - Add enough water to make it wet and mix. It should be like wet clay. (This freebases the DMT)
3 - Spread it out and let it dry completely.
4 - Dissolve it in acetone and filter out the solids. (Freebase DMT and other junk dissolves into the acetone)
5 - Saturate the acetone with fumaric acid.
6 - DMT fumarate precipitates out of the acetone. (Some other junk might also precipitate out the first time)
7 - Mix DMT fumarate with 1 part calcium hydroxide.
8 - Add enough water to make it wet and mix. (Freebase the DMT again)
9 - Spread it out and let it dry completely.
10- Dissolve it in acetone and filter out the solids. (At this point only alkaloids like DMT should dissolve)
11- Evaporate the acetone to get nearly pure freebase DMT.

Very interesting…SWIM will try that when he has some free time! I AM VERY EXCITED!!!!!8)

That looks very possible if those test results are accurate. That above tech works for bufotenine if citric acid is used. But to my knowledge, no one has tried that tech with fumaric acid.


As for dosage, 125 mg is a typical dose for snorting DMT. It should be very fine powder, not chunks.

What was the body load like that you experienced?
 
SWIM has to wonder how well the DMT-fumarate absorbs through the mucus membrane. Is there much throat drip? The reason SWIM wonders this is because of the high dose required for breakthrough. SWIM understands that a salt could never be as potent as the freebase, but so far it looks like so much sacrifice for very little benefit. SWIM would imagine that reducing the dose for insuffulation with an MAOI in one's system would work just as well as a larger dose on it's own. SWIM also wonders how this would stack up against encapsulating DMT-fumarate, pharmahuasca-style w/ MAOI. Or how about DMSO?

This is extremely exciting, but SWIM thinks the fumarate form probably has its own character; a tweaked method of ingestion seems to be in order.

Thanks for your work! SWIM can't wait to see how far this can go.
 
The convertion of freebase to a salt is pursued for meir reasons than insufflation alone. A major reason for SWIM is investigating all these funny little properties of dmt that make him experience what pure science feels like. Apart from insufflation however dmt fumarate is supposedly very stable and thus an excellent way of storing dmt (in case one has fairly large quantities). Or, as in the case above and below pursuing one thing may give inspiration for other aspects of dmt work, i.e. extractions)


69ron writes of some really good ideas! I was also thinking of a possibly simpler method:

1) acid extraction of MHRB. Your acid is FUMARIC ACID, so you convert all dmt to fumarate salt
2) boil down the extracts to a very very low volume.
3) add excess of acetone and cause precipitation of fumaric acid and DMT fumarate
4) collect precipitate and freebase it

SWIM would like to test the solubility of dmt fumarate in 90%, 80%, 70% etc acetone (the rest being water and/or fumaric acid solution) to see whether this is a viable strategy.

Or, even even better:

1) extract MHRB with acetone and filter off all pieces. (soxhlet should work miracles here)
2) (optional)evap to a managable volume.
3) add excess fumaric acid.
4) see the beautiful precipitate falling.
5) freebase it

69ron, can your friend or anyone else test whether the fumarate salts of other psychoactive alkaloids (i.e. 5meodmt and jungle spice) show similar acetone insolubility?
 
Ronue said:
69ron, can your friend or anyone else test whether the fumarate salts of other psychoactive alkaloids (i.e. 5meodmt and jungle spice) show similar acetone insolubility?
Click to expand...

Yes for bufotenine (5-HO-DMT), but not right now. His lab and several other adjacent rooms are being remodeled. The floors are being replaced, walls are being moved, new pipes are being put in, new sinks, everything is under construction...it is a mess! SWIM can't do any experiments until the construction is complete. Maybe two weeks more to go and it should be done, well most of it anyway.

I would assume that all of the citrates that are insoluble in acetone would also be insoluble as fumarates. Fumarates are in general less soluble than citrates in all solvents. If DMT fumarate is really insoluble in acetone as your tests show, I am willing to bet that 5-MeO-DMT, "Jungle Spice", bufotenine, and all the N-Oxides are also insoluble in acetone as fumarates.

Once SWIM’s lab is useable again, he can very quickly test this out with bufotenine. He’s been dying to know if bufotenine fumarate is a solid, because bufotenine citrate and bufotenine HCl are clearly not solids (they are goo like DMT citrate and DMT HCl).

SWIM no longer has any pure 5-MeO-DMT to play around with. He doesn’t have “jungle spice” either.

SWIM has lots of DMT to play with though.

SWIM was playing around with the idea of salting out DMT HCl from mimosa using JUST WATER, HCl, and salt. SWIM found out that it works and was excited to refine the tech, but had to stop because of the construction.

SWIM’s ultimate goal is to find an extraction tech that works for DMT that uses no messy emulsion plagued A/B extraction steps, no dangerous solvents (acetone is naturally found in the human body), and is efficient. The salting out of DMT HCl from water and table salt is a great new find and SWIM is excited about that. The yields were low, but SWIM’s mimosa might have been poor quality. It was cheap after all.

SWIM likes acetone. It evaporates fast, distills fast, is naturally present in the human body, and is very cheap and easy to get. If an acetone based tech for DMT could be had that is easy to do, it could greatly help out lots of people. And if sodium hydroxide could be avoided, that’s even better. Sodium hydroxide is almost impossible for lots of people to buy now in many places around the world. Calcium hydroxide is as strong of a base as sodium hydroxide is, but not as water soluble so it can’t be concentrated enough to reach a pH higher than 12.4. This makes it safer to use. Calcium hydroxide is also sold for cooking and is generally easier to get than sodium hydroxide. This is why most of SWIM’s techs use calcium hydroxide. The other base SWIM uses a lot in his techs is sodium carbonate which is also easy to get and much safer than sodium hydroxide.



Here’s another theoretical idea. I believe that DMT acetate is soluble in acetone (I know it’s soluble in DCM). One could extract DMT acetate from mimosa by using vinegar. Then evaporate the vinegar. Once completely dry, dissolve it in acetone, and then add fumaric acid. Fumaric acid will convert the DMT acetate into DMT fumarate and it should precipitate out of solution.

Of course this all assumes that DMT acetate is soluble in acetone and that the DMT present in the plant can be converted to DMT acetate. If it’s present as freebase then there’s no problem, but SWIM’s tests show its present as some sort of salt, not freebase, because it is easily extracted into pure water from the plant. SWIM has no idea what salt form its present as. Maybe DMT carbonate? Is that possible? I know that mescaline carbonate exists (mescaline has a pKa of 9.56) and bufotenine carbonate exists (pKa of bufotenine is 9.67), but I don’t know if DMT carbonate exists (DMT has a lower pKa of 8.68 and that might be too low).

NOTE: bufotenine carbonate forms from freebase bufotenine if it's exposed to air for too long. This causes it to turn dark brown, with a shiny tar like look, and all the powder gets stuck together as one hard lump. Bufotenine carbonate is more water soluble and less hallucinogenic than freebase bufotenine. So if this happens, you’ll need to freebase it again to regain the potency. Another problem with storing bufotenine is that it also forms bufotenine n-oxide which is barely hallucinogenic at all.
 
All these are very promising indeed, SWIM's head is burning with ideas!!!

Should a new topic be started discussing alternative (and more safe) methods of spice acquisition?
 
That's not a bad idea.

The world needs some less toxic safer extraction techs for DMT. Most popular DMT extraction techs involve hot naphtha (an extreme fire hazard) and sodium hydroxide (a very dangerous chemical). I know many people that wouldn't consider having naphtha in their house because it's so flammable. And then there’s the fact that sodium hydroxide can eat through your flesh, not to mention it’s now nearly impossible for some people to get.

I think it’s really time that some alternative techs are created for extracting DMT. Something like the salt based tech for extracting harmine would be nice. That tech requires no dangerous solvents or chemicals. None at all. And it works really well.
 
What would you use to get DMT base from the DMT fumarate? That would be a good extraction tech, kind of a way to ensure that there would be less dangerous impurities. Extract from bark, precipitate with fumaric acid, convert to base. Or would that be difficult because the acetone/fumaric acid ratio?
 
That is fairly easy for SWIM; DMT fumarate can be dissolved in water, 5ml are then enough to dissolve 500mg dmt fumarate, then add base and see the solution going milky (the "sperm reaction" due to the viscosity and appearance of the resulting liquid), then wait for this insoluble material to sediment (1-2 days). SWIM's lucky enough to own a centrifuge which speeds up this process in 10 minutes!

SWIM is also trying to develop a centrifuging system for precipitating freebase out of basic solutions using the home's centrifuge that almost all people own: the washing machine.
 
I didn't know freebase DMT would settle down out of the water after 1-2 days. Are you sure about that?

Man I love your ideas. The washing machine is indeed a centrifuge, especially the one I own. That sucker spins REALLY FAST. That gives me some new ideas:)
 
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