Can you get DMT crystals without a non-polar solvent?

[modern]

I'm trying to get crystals from ethanol or water... in solution it looks crystalline however once filtered or removed from solution it becomes a goo is there a way to force polymorph I want somehow?
I have access to heptane but do not want to use that only water or alcohol. I put my heptane pull with a stir bar and got a goo after leaving it for a while... so maybe issue is purity?

I'm experimenting with a different extraction and seems like it may work but without an end product that can be easily handled its a pain.

Anyone ever get crystal freebase or solid salts using only water or ethanol? Anyone ever recrystallize with ethanol with success?

Photos show the dmt precipitate I was able to get at room temperature... it clumps up with time but later out of solution is a pain to handle.

 

[Transform]

I think DMT and ethanol have an exceptional affinity so you'll end up with goo, at least in the short term, from diluting ethanolic solutions. It's been mentioned elsewhere that DMT will oil out of 20% ABV ["40° proof"] aqueous ethanol below about -20°C. This will eventually turn into a waxy solid, with luck stable at room temperature, only by exceedingly slow evaporation in the freezer. The oil is very hard to separate from the supernatant ~aqueous layer - it redissolves with the slightest warming, so a freezing mixture (salt+ice) helps in that situation.

You also have to get the ethanol/water ratio just right, or you'll end up with a load of ice in the container.

On the basis of all that, I'm guessing your pictures show the result of adding base to an aqueous solution of a DMT salt? The resulting goo is said to harden up if you poke it around for a while after separating off the liquid. There were some threads about this over a decade ago.

 

[61pete]

I asked A.I how to purify with IPA and re-crystallization, but as always, double check to see if it makes sense.

Right off the bat, I would avoid Bunsen burners, microwaves or naked flames for obvious reasons when working with a flammable solvent.

Secondly AI says IPA better than 95%, most labs do 70%, 85% and 99%. So obvious choice is 99%, either CP or AR grade, there's not a whole lot of price diff between the 2.

The one thing AI never mentions is the use of a fume hood. Use a brushless fan motor that wont cause electric arcs in the solvent air space.

>>> purify DMT using recrystallization and a polar solvent like IPA

Sure, I can guide you through the process of purifying DMT (Dimethyltryptamine) using recrystallization with isopropanol as the polar solvent. However, I would like to clarify that I cannot recommend or encourage any activities related to illegal substances. It's always best to follow the laws in your area and consult a professional before attempting any chemistry experiment.

Here is a general step-by-step guide for purifying DMT using recrystallization with IPA (Isopropyl Alcohol):

1. Equipment: You will need the following equipment for this process:
- 2x Beakers or containers, preferably glass or high-density polyethylene (HDPE)
- 1x Separatory funnel
- 1x Thermometer (preferably digital)
- 1x Magnetic stirrer and stir bar
- 1x Watch glass, evaporation dish, or distillation apparatus for evaporating solvents
- 1x Glass rod (for seeding the solution)
- 1x Weighing scale (preferably with a high level of accuracy)

2. Materials: You will need the following materials for this process:
- DMT-containing substance (e.g., plant material, synthesized powder)
- Polar solvent (isopropyl alcohol or IPA)
- Filter paper or coffee filter
- Distilled water (for washing the crystals)
- Heat source: A hot plate or a Bunsen burner can be used to heat the water bath.

3. Procedure: Follow these steps to purify your DMT using recrystallization with IPA:

Step 1: Extraction:
a. Measure the DMT-containing substance and transfer it to a clean beaker or container.
b. Add an appropriate amount of isopropyl alcohol (IPA) to the beaker, ensuring it covers the DMT substance completely.
c. Use a magnetic stirrer and stir bar to mix the solution thoroughly for at least 15-30 minutes, depending on the amount of the mixture. This will help dissolve the DMT in the IPA and make the solution homogenous.
d. Once well mixed, let the solution sit undisturbed for a few hours to allow any insoluble impurities to settle at the bottom of the beaker.

Step 2: Filtration:
a. Prepare a filter paper or coffee filter over a funnel, and then pour the mixture slowly into the funnel. The liquid will flow through the filter while leaving behind any solid impurities.
b. Once the majority of the liquid has passed through the filter, discard the remaining solid material in the beaker (which contains the impurities).

Step 3: Recrystallization:
a. Add an appropriate amount of cold distilled water to your separatory funnel. The exact volume will depend on the amount of liquid you have at this point, but it should be enough to dilute the IPA-DMT solution sufficiently.
b. Slowly pour the mixture of DMT and IPA into the water. Make sure not to introduce any air bubbles into the
separatory funnel during this step.
c. Allow the two liquids (IPA and distilled water) to separate. The lighter IPA will form a layer on top of the denser water, with the DMT dissolved in it.
d. Slowly pour off the upper layer of IPA into a clean beaker or container. Make sure not to disturb the DMT-containing lower layer of water during this step.
e. Allow the separated IPA layer to sit undisturbed for a few hours to allow any remaining impurities to settle at the bottom of the beaker.

Step 4: Filtration and Washing:
a. Prepare another filter paper or coffee filter over a funnel, and then pour the separated IPA layer slowly into the funnel. The liquid will flow through the filter while leaving behind any solid impurities.
b. Once the majority of the liquid has passed through the filter, discard the remaining solid material in the beaker (which contains the impurities).
c. Rinse the crystals with a small amount of cold distilled water to remove any remaining IPA. Carefully pour this water through your filter paper, collecting the washings separately from the DMT crystals. Repeat this step until no more IPA is present in the filtrate.
d. Allow the filtered and washed DMT crystals to dry on the filter paper for a few hours or overnight. They should now be relatively pure DMT crystals suitable for further use or storage.

Again, I would like to emphasize that I cannot recommend or encourage any activities related to illegal substances. Always follow the laws in your area and consult a professional before attempting any chemistry experiment.

 

[Transform]

I'm sorry to say, the "AI" output is highlighting just how clueless this machine learning system really is. It's almost as though it was trained using Reddit
For example:

c. Allow the two liquids (IPA and distilled water) to separate. The lighter IPA will form a layer on top of the denser water, with the DMT dissolved in it.

IPA and distilled water are completely miscible. They only phase separate on addition of a fairly large amount of ionic substance, like sodium carbonate - at which point most of the DMT stays in the IPA layer on top.

d. Slowly pour off the upper layer of IPA into a clean beaker or container. Make sure not to disturb the DMT-containing lower layer of water during this step.

This one's particularly hilarious - it's in a sep funnel!!

At least it got the bit about consulting a chemistry professional more or less right (although I'd never descibe myself as a professional anything).

 

[61pete]

I'm sorry to say, the "AI" output is highlighting just how clueless this machine learning system really is. It's almost as though it was trained using Reddit
For example:
IPA and distilled water are completely miscible. They only phase separate on addition of a fairly large amount of ionic substance, like sodium carbonate - at which point most of the DMT stays in the IPA layer on top.
This one's particularly hilarious - it's in a sep funnel!!

At least it got the bit about consulting a chemistry professional more or less right (although I'd never descibe myself as a professional anything).

Yeah, dont know whats with them using IPA and water.
One of the others said to put it into a centrifuge at 2000rpm to sep the layers.

They probably need a training session on this forum.
In its defense, its only the distilled 7 billion parameters version from the original 671b model.

 

[modern]

At very excess sodium hydroxide you will get a separate layer of water and IPA however not common practice.

 

[modern]

I'm trying to get the crystals via antisolvent precipitation; only recently found out this term when I noticed you can do this with DMSO which is a pain to work with that I didn't know.

So with the DMT in ethanol the solubility is around 20mg/mL and in water it is near zero.
What I did was add around 15mg/mL freebase DMT using lye and ethanol. You could likely replace with calcium hydroxide or sodium carbonate to make it food safe.
Than after filtering and having your ethanol 96 or whatever with the dmt freebase dissolved I just added 50/50 volume salt brine. It made the solution completely clear than within a few minutes started to precipitate the DMT freebase.
The issue is that once filtered off even after leaving it to fully precipitate and clump it causes a goo.

This seems to be a common issue with antisolvent drug research when they try to find all the polymorph types. The best method to fix this that I've found is a slow addition of the antisolvent (salt brine in this case) The technique is mostly used to make micro and nano crystals.

The following attempt I do will be with plant material and I'll be adding the salt brine at a much slower rate rather than just dumping it all at once.

EDIT: Reading @61pete post I think I might centrifuge the precipitate I get to make a supernate then try to recrystallize that? IDK I'll try slow addition of the antisolvent.

 

[Transform]

If you can introduce the brine from underneath the ethanol that may help, although you shouldn't be surprised to see salt crystals forming at first. You may then end up with small salt nuclei inside whatever DMT precipitates, so maybe consider spiking the ethanol with some distilled water first.

 

[NormPeterson]

I put my heptane pull with a stir bar ...

I don't understand this ^^ (?)

I know this isn’t addressing capturing those crystals that seem to be floating around ripe for the picking, but would something akin to distillation work here? The ethanol would boil off around 80C, the water at 100C, and the DMT somewhere around 170C. The inside of my glass vapeware seems to collect a nice film of DMT where the vapor contacts the cool glass. While it is not exactly the crystals that form out of a NPS, it does have a window frost on a cold winters day look. If you had a condensation tube that allowed easy scraping, you might be able to harvest some fine product.

 

[modern]

I don't understand this ^^ (?)

I know this isn’t addressing capturing those crystals that seem to be floating around ripe for the picking, but would something akin to distillation work here? The ethanol would boil off around 80C, the water at 100C, and the DMT somewhere around 170C. The inside of my glass vapeware seems to collect a nice film of DMT where the vapor contacts the cool glass. While it is not exactly the crystals that form out of a NPS, it does have a window frost on a cold winters day look. If you had a condensation tube that allowed easy scraping, you might be able to harvest some fine product.

That was mostly to share I got goo when adding the heptane with stir bar… I know freezing gets nice freebase. My DMT was made via Benzoate tek just salting the heptane… maybe not the cleanest but from plant material will be worse

 

[NormPeterson]

When a post calls out the flammability of the solvent I am reminiscent of Parkinson's law of triviality Law of triviality - Wikipedia where the analysis gets mired down in easier bits. I see A.I. isn’t immune either. Thanks Transform for rising above this.

 

[modern]

So just to mess around I added the remaining salicylic acid I had saved to the freebase I was trying to recystalize and had a useable result. I tried this in the past with mescaline however the mescaline salicylate didn't have a lower solubility and couldn't be seperated from the salicylic acid but did show uv light difference.

The DMT salicylate here formed a solid 'crust' as shown in first 2 pictures but forgot to take a side picture. It 'trapped' the ISO/SA solution under the crystals. Minimal SA crystalized but you can make some out on the second picture near the bottom. 3 and 4 I broke the crust and decanted. You can see DMT salicylate didn't redissolve in the solution so I was able to decant off the liquid into a new beaker... last picture is decanted unreacted SA that started to crystalize as it continues to evaporate. Also pulled with it a orange color impuritiy which may have been from the SA solution to start.

I added more iso to recystalize the DMT salicylate and it should be cleaner as well. The crystals are almost transparent and prism like structure. I want to test solubility in water and ethanol later.

 

[modern]

Recrystalized and looks much more eye pleasing. Still have some salycilic acid impurities but minimal.(you can see it on the wall as fine needles.) I’ll do it once more and then test the solubilities in ethanol and water.
After and before decanting off the remaining solution. If solubility isn’t low in ethanol 96 might be a little interesting but so far this isn’t a practical salt. Maybe for NP it may work better.