White DMT crystals -> DMT Fumrate Goo?

[Levanah]

Hey fellow travellers,

I just converted 1g white freebase DMT with this tek:

Here’s the quick tech:

1) Completely dissolve 1000 mg of freebase DMT in 50 ml of acetone.
2) Completely dissolve 309 mg of fumaric acid in another batch of 50 ml of acetone.
3) Mix for 1 minute and evaporate at room temperature to give DMT fumarate.

Instead of acetone I used IPA.

What I got out is DMT fumarate goo. I have never seen fumarate salts settle as goo before.

I don't mind working with goo for my purposes. I like goo.

But actually I wanted to achieve easy to handle fumarate salts.

Any idea why it turned into goo?

With my pull 6+7 I yielded 300mg (the last 10% yield of 250g MHRB) of a similar looking freebase goo.

I scraped of 99% of that goish freebase from my evaporation dish and used the same evaporation dish for the evaporation of the DMT Fumarate IPA solution.

So why did my DMT fumarate turn to goo?

Was it

1) the high room temperature (23-24 °C) and the fast evaporation of IPA
2) or maybe due to the 1% rest of the "freebase goo" which dissolved 100% into the IPA, when I put the IPA into the evap dish?

I can hardly imagine both, after all, even the evaporation with just petroleum ether (which I used for the extraction) yielded white and brown freebase crystals even with rapid evaporation.

But maybe it's because petroleum ether can't hold much dmt freebase and crystalizes better as the freebase crystals are crashing already out before full evaporation. Maybe thats it?

Just as a sidenote: For good measure, I calculated 10% more fumarate acid (so 340mg fumaric acid for 1g white freebase DMT).

Thanks,
Levanah (Hebrew: moon)

 

[Dirty T]

Was the IPA dry? Goo is the result of moisture. Either where you dried it was very humid or your IPA has water in it. 1 drop of water in a quart of Naphtha can turn the entire tray to oil.

 

[Levanah]

Was the IPA dry? Goo is the result of moisture. Either where you dried it was very humid or your IPA has water in it. 1 drop of water in a quart of Naphtha can turn the entire tray to oil.

1. Was the IPA dry?

Yes it was freshly opened 99,99% IPA.

2. Was my room very humid?

Maybe thats it! I evaporated the IPA in a room with all windows open and directly under a big open window over night.

Moisture from outside air could have gotten in there.

In the morning I saw drops of water in the evap dish.

As I said - I like goo and don't have problems with goo. We all know goo is good.

That being said, as everything is still in the evap dish, what would be your recommendation to convert the goo to solid DMT fumarate crystals? (doesn't need to be perfect)

Maybe another shot of IPA and evaping it again in another room with hopefully less moisture? Or buying fresh acetone and re-evap?

Can dry (closed) IPA possibly go bad (can it draw water?) over years of storage?

Another question:

As I'm fine with goo I am NOT fine with loss of yield / loss of good spice.

But since only by evaporation no DMT can disappear / get lost I could theoretically do a thousands of re-crystallization attemps and not lose any yield, right?

 

[downwardsfromzero]

If it's any consolation, the goo can turn to crystals, especially if you store it in a desiccating chamber of some sort. Unfortunately, even then it's not as lovely as precipitated sparkles. Something you might want to try is recrystallising DMT fumarate from boiling IPA.

Besides moisture, having taken a look at the method you outlined, Levanah, the fact that it says to evaporate all the solvent is kind of a red flag as far as purity goes. The point of FASA precipitation is that the DMT fumarate is insoluble. The fumarate crystals settle out of the mixture and can be recovered by decanting or filtration.

When you evaporate all the solvent two or three things will occur. Firstly, any soluble impurities will be deposited on the fumarate crystals instead of being washed away like if you had removed the crystals from the solution. And then it comes back to moisture: the residual water will become concentrated and eventually soak into the fumarate - and IPA is fairly hygroscopic so it's pulling water out of the atmosphere as well.

One other factor to consider is the differing solubility of fumaric acid in various solvents. There's the FASIPA Method, but that goes nowhere near quantifying the solubility of fumaric acid in IPA. Benzyme estimates it as being "difficult" - again, no quantification. This post by Luz brings us a little closer to some numbers: "As I understand it, the solubility of fumarate in acetone, in water, and in IPA are all very similiar, between .6 and .7 gr per 100 ml". Then here, some one has made a nice generic explanation of the FASX process and mentions, "The solubility of FA in Acetone and water is 6mg/ml and in IPA 5mg/ml" - but I'd say that IPA figure is on the low side.

While going through the search results, this also came up in a post by Luuk: "A good method for purifying is to dissolve freebase in IPA, add straight fumaric acid (no FASI!), and stir good. This causes an instant precipitation of small but pure DMT fumarate crystals. The DMT fumarate formed is contaminated with fumaric acid but this can easily be removed by dissolving the DMT fumarate in water." So, no need to worry about the precise figures after all, perhaps. Except Endlessness provided a link to some definitive data here. It turns out that the solubility in various solvents increases in the order: water, acetone, n-propanol, ethanol, IPA.

Propan-2-ol

T/K x1·10³ 100(x1 - x1calcd)/x1

279.00 10.92 -11.1
285.00 13.78 -3.90
291.00 16.85 0.30
297.00 20.23 3.05
303.00 23.59 3.42
309.00 27.25 3.38
315.00 30.97 2.17
321.00 34.92 0.56
327.00 39.10 -1.33
333.00 43.48 -3.58
342.00 53.79 -0.81
351.00 65.62 1.27

Temperature in K in the left column, solubility is presented as a mole fraction in the middle column. Converting mole fraction solubility into more everyday kind of units requires a bit of basic arithmetic and the MW of fumaric acid and IPA, plus the molar density of IPA. I'll leave that one as a challenge.

Just remember, it's not really recrystallisation in the strict chemical sense if you evaporate all the solvent.

 

[Levanah]

If it's any consolation, the goo can turn to crystals, especially if you store it in a desiccating chamber of some sort. Unfortunately, even then it's not as lovely as precipitated sparkles. Something you might want to try is recrystallising DMT fumarate from boiling IPA.

Besides moisture, having taken a look at the method you outlined, Levanah, the fact that it says to evaporate all the solvent is kind of a red flag as far as purity goes. The point of FASA precipitation is that the DMT fumarate is insoluble. The fumarate crystals settle out of the mixture and can be recovered by decanting or filtration.

When you evaporate all the solvent two or three things will occur. Firstly, any soluble impurities will be deposited on the fumarate crystals instead of being washed away like if you had removed the crystals from the solution. And then it comes back to moisture: the residual water will become concentrated and eventually soak into the fumarate - and IPA is fairly hygroscopic so it's pulling water out of the atmosphere as well.

Thanks for all ya advice, I've learned a great deal from your post!

Afterall, my problem has been completely solved. I just let the evaporation dish dry for a few days and retrieved perfectly fine fumarate powder.

I know that evaporating all solvent is kind of a red flag. I just want to clarify at this point that the primary white spice was obtained from a freeze-prep.

So it was really just moisture.

Recrystalising DMT fumarate from boiling IPA is a great suggestion.

I would or will try it if I'm ever interested in crystal eye-candy.

But for now, I'm very satisfied with the obtained end product - it's perfect for my purposes.

 

[downwardsfromzero]

Glad to hear that it turned out well in the end. Patience is often the key.

A bit annoying that they put the embossed log on the inside of the dish, eh? :lol: