Hello,

SWIM is looking to "streamline" the extraction process with as few solvents and steps as possible, while retaining the quality and yield. He has a sufficient knowledge of organic chemistry, but has yet to "apply" it to something useful.

So SWIM has supplied me with the following schematic of sorts to get input. It seems almost too simple, but everything seems to check out relatively well as far as chemical theory is concerned. Right?

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Simplest Acetone Extract

1. Basify

I've decided to cut out the defatting process due to the low lipid content of MHRB powder, and because the salt precipitation of the alkaloids into their fumaric complexes isolates them from any fat contamination anyways.

So to basify the MHRB, add enough water to a 1:1-1:5 ratio of a water soluble hydroxide salt (NaOH, KOH, CaOH) and powdered MHRB to make a paste (or add a solution of water and a pure alcohol to decrease evaporation time). Wait until the paste is completely dry.

If you cannot find a hydroxide salt to purchase, one can make some by extracting it from wood ash. Wood ash is mostly potassium hydroxide (very slightly less basic than NaOH, but still good enough) with a bit of sodium hydroxide mixed in. The age-old method is to use a big barrel, put straw or dry organic matter at the bottom of the barrel, and pile in the wood ash on top. Then fill in the water and allow it to percolate through the ash. The straw and organic matter should filter out most particulate matter. Draw off the water from the bottom of the barrel. The water is now highly basic. Use this to mix with your MHRB, or dehydrate to leave crystalized hydroxide salts. Other methods call for things like coffee filters or just allowing the ash to settle in solution, so one can draw off the water from the top.


2. Acetone!

Add enough anhydrous acetone to inundate and have excess in the containment vessel (glass only). Wait until the particulate matter settles and decant & filter acetone. The freebase alkaloids have now passed into solution. The solution will probably be cloudy and have impurities at this point.


3. Salt Precipitation

Slowly add Fumaric Acid Saturated Acetone (FASA) dropwise into alkaloid-acetone solution to precipitate out alkaloid salts. Wait until salts have settled and decant remaining acetone solution. Wash salts with additional acetone until any lipids or other impurities are gone.

Convert to freebase using NaCO3 (1:1). Mix salt and base together, add enough water to make paste. Allow to dry. Add acetone to dry mixture to draw off freebase and leave excess NaCO3 and Fumaric Acid. Decant acetone and allow it to evaporate. Freebase alkaloids are left.

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So basically that's it. I figure even if someone were to use something fattier than MHRB, the precipitation of indoles would prevent most other impurities (tannins, lipids, phenols, etc) from being in the final product. Now because the precipitation tends to be non-selective as far as alkaloids are concerned, the resulting product would likely be "jungle spice". But if one were to do a non-polar wash, the desired alkaloids could be obtained.

This process seems so much more easy and safe than using caustic chemicals and dangerous hydrocarbons. Is there any visible downside to any of you?

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Results of the Above Tek
So if you read through this thread, you'll notice that nothing precipitated out of the final acetone solution. I have ruled out the presence of water (which would keep fumarate precipitates in solution), so the only other reason for the lack of product would be too low of a pH during the basifying stage. For this reason, I have adjusted the above tek to use a more basic hydroxide salt instead of a carbonate. If someone wishes to attempt the new version, feel free to do so. I am going to do rebasify my left over MHRB and do a non-polar pull to verify that the alkaloids are, indeed, still present.


-- Wanderer

Im not aware of anybody trying such a method. It could work.

But acetone will pull a lot of impurities in the first step, so Im not sure how much this will affect fumarates precipitaton. Maybe other impurities will precipitate together, maybe it wont precipitate at all if for some reason impurities prevent precipitation from happening.

Im neither sure how strong sodium carbonate will be. Maybe a stronger base is necessary, but im not sure how reactive acetone is to hydroxides?

In any case I think its worth a try (unless someone comes up and says they did and it didnt work). Do a small batch first and dont throw anything away.

Also for the conversion to freebase, you could try doing the slow water conversion instead, could potentially get you a purer product.

Good luck and dont forget to let us know if you do try it (Whether this works or not, I like the experimenting spirit, keep trying to think out of the box )

Good call on the cold water technique!

Well I can't think of any organic compounds that would form any sort precipitate with fumaric acid beyond indoles and some other alkaloids. Tannins and phenols should remain in solution, and any lipids won't react with acids. Additionally, washing the alkaloid salt numerous times should purify it relatively well.

Regarding the basicity of NaCO3 (around 11.8 pH I believe), I think it should sufficient since the pH of freebase DMT is below 9 (8.7?). Additionally, too high of a pH might dissociate salts of other compounds that aren't desired.

In any case, SWIM will be sure to provide me with some results soon.

-- Wanderer

An update!

So all the precursor reagents were made today, which I will detail below:

Chemical Stock Creation

Sodium Bicarbonate [Na2HCO3] --> Sodium Carbonate (Na2CO3)
Thermal dehydration decomposition of Sodium Bicarbonate (baking soda) to Sodium Carbonate (soda ash) for use as base (pH of 11.6, sufficient for freebasing most tryptamine alkaloid salts -- tannates, etc). The reaction is relatively simple:

2(Na2HCO3) + Heat (above 70 C) ---> Na2CO3 + H20 + CO2

Process: Arm & Hammer brand baking soda and a stainless steal sauce pan were used. The baking soda was put in the pan, which was placed on a burner. As it began to heat, steam would rise off, indicating decomposition. The dry compound was stirred with a stainless spoon; as it was stirred, small "eruptions" of gas could be seen making holes in the powder. The powder was stirred until no more steam could be seen rising, and the overall texture had changed to that mirroring Na2CO3 (fluffier, different shade). This was set aside to rest and cool in a mason jar.

Magnesium Sulfate [MgSO4 * 7 H2O] --> Anhydrous Magnesium Sulfate (MgSO4)
The purpose of creating this compound was to desiccate (dry) the acetone to be used for extraction. Because we will be precipitating out the fumarate salt of DMT (and related alkaloids), the precipitates will be soluble in water. If an appreciable amount of water is present in the acetone solution, the alkaloids will be stored in the water fraction (acetone and water are miscible -- they mix homogeneously). Dehydrating Magnesium Sulfate (Epsom salt) renders it a desiccating agent. It forms stable hydrate complexes consisting of 7 water molecules, and so is highly hygroscopic (water-seeking).

Reports can be found that claim it does not "dry" acetone well, but shake up the can enough and wait a day, and it should remove most water. If one is extremely paranoid about yield loss, allow the remaining acetone after salt-precipitating to evaporate, re-basify the remaining sludge, and extract with a non-polar solvent (Naptha and d-Limonene seem to be the top contenders, though Toluene and Xylene are also used -- keep in mind the latter of these four are both carcinogenic, and have been linked to the development of leukemia and other systemic cancers; most distilled fossil hydrocarbons tend to do that).

The reaction(s) is simple, but has two main steps:

(MgSO4 * 7H2O) + Heat (150 C) ---> (MgSO4 * 1H2O) + 6 H2O (steam)
(MgSO4 * 1H20) + Heat (200 C) ---> MgSO4 + H2O (steam)

Process: The same stainless saucepan used to create NaCO3 was cleaned and reused to dehydrate Magnesium Sulfate. Crystals were poured in (roughly 250 grams) and distributed evenly to a depth of roughly 1-2 cm. Heat was applied via an electric burner. Within a few minutes, visible "water" could be seen collecting interstitially between crystals as it was liberated from the hydrate complexes. "Crackling" noises could then be heard as it began to evaporate. Stirring could not be readily achieved due to the hardening of the crystals caused by the liberated water, so the saucepan was left on high heat.

Over the course of about 20-30 minutes, the "clearness" of the Magnesium Sulfate was no longer visible. Instead, a chalky, opaque residue was left -- this is anhydrous MgSO4. It is hard after this process, so it took some "grinding" with the bottom of an old mason jar to powder it. While still hot, the powdered MgSO4 was placed into a mason jar and sealed to prevent it from taking up atmospheric water. After it had cooled, a liberal amount was placed into the acetone, which was then shaken and left to sit for 24 hours (probably excessive).

Root Bark Basification

The newly created NaCO3 was then used to create a saturated solution (roughly 400 mL worth). NaCO3 was slowly added to purified water until no more would dissolve (visible, large NaCO3 crystals should form at the bottom of solution when maximum solute content has been achieved). This should have a pH of roughly 11.6 at 20 degrees Celsius.

This solution was then added to roughly 150 grams of powdered MHRB. After a good amount of stirring, the pink powder mixed with the basic solution, quickly turning blackish/greenish, signifying that the solution is, indeed, sufficiently basic (a conversion of tannic pigments).

The smell is distinct -- it's highly reminiscent of "stink horn" mushrooms. Coincidentally, the goop created is similar to the goop atop a stinkhorn. It's an almost "spermatic" odor to my nose, and I'm sure a few men and women would have similar interpretations.

The root bark is then dried completely. DON'T HEAT above 80 degrees Celsius, or you may lose some of the freebased alkaloids which have developed a much lower melting point outside of their salt form. This is currently where SWIM is at in the process. He will report more as the process continues.

Until then!
-- Wanderer

Na2CO3 is poorly soluble in water and it takes large amounts to get to 11.x. Although it might work if you're aiming for paste.

Indeed, at 20 C one would need a minimum of 88 grams to achieve maximum solute content in 400 mL of water. But NaOH appears to be difficult to come by locally, and always runs the risk of attracting attention from undesirable authorities due to its other various uses. If Sodium Carb proves to be effective, it may help a number of others in similar situations.

A friend tried this, but with lime and acetone. It worked, but the results were poor. Low yield and very dirty. It took a lot of clean-up. To get a worthwile yield, you will need to do the basify and acetone steps several times, because one wash just won't do. All that water and acetone drying is time consuming, and you're going to go through a lot of acetone. You might want to take a look at some bufo extractions, which is what inspired me to try this. For step 2, the acetone wash, a THP setup would be more efficient than a simple soak and decant (soak and then THP is even better). It was interesting, but it was more trouble than lye, limo, and acetic, which has become my preference. FASA is cool too, but a real sep funnel makes the water washes so much easier. Water washes seem to get better yields, I can be more confident that everything is out of the limo. You can't re-FASA limo, but you can re-wash with vinegar all you want. A NP solvent transfer is so much better, IMHO.

But don't let me discourage you, I hope you get better results than my friend. The way you are documenting this is great!

Additional Update: Drying process continues. Added anhydrous MgSO4 to desiccate sludge, but it still requires additional drying. It has taken on a fluffy, whipped sort of texture.

Also, damon: Did your friend use a FASA precipitation to separate the product, or just evaporate filtered alkaloid-acetone solution?

-- Wanderer

YES! Someone is finally writing up a report for this method. I will be attempting this method for my next extraction most likely.

It was this method that originally got me thinking I could actually pull off an extraction. It was originally discussed in this thread: https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=24922#post24922

That thread is a bit muddled, certainly, but the tek is there. It's just no one has tried it, or at least no one has written a report about the results. I don't see why it wouldn't work, or why it would produce "dirty" spice if you perform it properly and use the FASA method.

Very interested to know the results. Do keep us posted!

Will do! The drying is almost complete. The anhydrous MgSO4 seemed to take some time to form hydrate complexes at 15 C, so I've put the mixture under a heating fan. It's now about the consistency of dryer dutch apple-pie topping. Pies sure are delicious

-- Wanderer

Evaporated acetone, then multiple acetic washes and then carbonate for base. It is very dirty after the acetone wash, since you're getting a lot of things you don't want. The only things being excluded would be salts and plant matter. Acetone is not very selective, hard to keep dry, and hard to get anything out of it without simply letting it dry up. Some kind of mini a/b is required, because the base at this point will taste so bad it would make me puke. I wouldn't even use it for oral. If you FASA the acetone, you will get dirty crystals, because you not excluding anything, like you would with a water wash. Rinsing with acetone will clean it up, but you will have acetone locked up in the crystals, and you'll need to do one or two water recrystals. It would be even better to do another conversion with water and acid to really clean it up (after FASA then carbonate). An NP solvent creates a "barrier" so that only certain compounds migrate, but since your not using that barrier you are going to spend more time cleaning up your results.

I love pie.

That's the one part that I thought would take the most time, is the drying. And making sure that you keep everything dry. Your understanding of chemistry is obviously far superior to mine, so I'm really excited to see where this leads and if this method is worth giving a try.

Really? Maybe I need to read more about solvents, especially acetone...

Yes, the crystals will contain a little bit of the solution they are formed in and a little of whatever else is in the solution. It might not smell like acetone at all, but once you dissove it in water, you will smell acetone. I don't think the acetone is becoming part of the crystal structure, but maybe the crystal can form itself around spaces that contain acetone, or binding somehow. These aren't going to be perfect crystals like you see in a geode, it would be more like a sparkly oily slush, if sparkly at all. Using acetone will give full spectrum too, so it would never really look like crystals. FASA on limo will get you fumarates with limo too, even after acetone washes, but the limo makes the crystals smell nice, so it isn't as important to clean up.

Thanks for the input damon!

Well the molar concentration of acetone in the fumarate precipitates will be virtually negligible. Additionally, the crystals can be heated past the boiling point of acetone to remove any trace of it. Unlike MgSO4, acetone doesn't form any sort of stable complex with indole salts (or pretty much anything else that I am aware of), and so little additional heat is required to remove it. It is chemically impossible for acetone to be "locked" up in indole structures, so given sufficient time, heat, or vacuum pressure, it will be removed. Like small particulates in soil (think clay), small pores in crystalline structures tend to hold on to solvents (like water) due to capillary and cohesive molecular forces. But given enough time, the volatility of the acetone will require that it completely evaporates.

Additionally, the point of using fumaric precipitation is to isolate tryptamine indoles from the lipids, tannins, and other phenols and proteins in the acetone. After filtering the acetone, the remaining compounds in solution should be those that are fully soluble in acetone. Once fumaric acid is added, it forms insoluble complexes with tryptamines, allowing them to fall out of solution. I am not aware of any other compound that fumaric acid will react with that will be insoluble in acetone, and so the insoluble tryptamine salts can be washed with clean acetone to remove any remaining soluble impurities.

Regarding basicity, the precipitation reaction removes the tryptamines from basic solution, so "taste" at this stage is irrelevant.

I expect the product to be a relatively pure and clean extraction of most indole compounds in the MHRB, which are mostly going to be the methylated tryptamines.

Time to get some coffee!

-- Wanderer

I don’t think that’s true. I’m not a chemist, but common sense suggests it’s not true. For example, when forming salt crystals (NaCl) in water solution, there is no water “trapped” in the crystals. Also, if solvent was commonly trapped in crystals during crystal formation, then crystallization wouldn’t be a very good method of purifying substances. Re-crystallization is a method used to purify many substances. If it excluded some impurities and introduced new ones (the solvent) then what good would it be?

I also state this from experience. After thoroughly drying crystals crystallized in naphtha or heptane, the crystals don’t have the slightest odor of solvent, even when crushed or powdered. (And the human nose is a fairly sensitive chemical sensor!)

Yeah, I'm with you gibran. A solvent cannot form bonds with an insoluble salt... in fact, I don't think it forms any strong chemical bonds with anything but itself. Water can form hydrogen bonds and hydrate some salts, but this isn't the case for acetone.

So the basified MHRB powder has been dried and placed in roughly 1.2 L of acetone (probably excessive), leaving a clear fraction of roughly 300 mL on top. This clear fraction will be siphoned off and filtered, and then precipitated. The fumaric acid still needs to be procured, so this last step will take a bit longer still.

-- Wanderer

I'm also with you gibran. I didn't think solvents could be "locked up" in the crystals like that. Although my understanding of the chemistry is admittedly far less than The Wanderer and yourself.

@Wanderer - There's a good, cheap source for fumaric acid in the suppliers section. It's where I purchased mine from, very good price. I can't mention the name here, PM me if need be.

Also, 1.2L does sound excessive for just 150g of bark. I'm wondering what the minimum amount necessary would be...although I intended to attempt my first extraction with a smaller amount of bark (probably 50g). I have a lot of acetone, it's just I wouldn't want to use it in excess if it wasn't necessary. Waste not want not!

damon is correct,
inclusions of some solvent are going to occur(unless the crystal formation happens in an absolutely perfect environment). this happens in nature as well.

if you precip from acetone, or any dirty solution there will be trace inclusions in the crystal matrix. it is unavoidable. the larger the crystal, the more inclusion typically
so,
precip crystals, then clean by grinding and washing- or redissolve into water, etc

edit: good work W, and welcome

Reading an excerpt from this book I learned that crystal inclusion can and does occur, but tends to occur only under particular circumstances:



So it seems that supersaturated solutions and rapid crystal growth make inclusions more likely to occur. I wonder how much solvent is actually trapped in crystals of the type that we grow? My guess is that the amount is negligible under typical conditions.

I just powdered some crystallized DMT and didn't smell even a hint of solvent, but I suppose that to be absolutely safe, it’s reasonable to re-dissolve in solvent and evaporate.

yeah, inclusions rarely make up a large percentage of the crystal, but often add colored impurity to the crystal.