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5-MeO-DMT recrystalization + Crystals at the µ-Scale Options
 
Brennendes Wasser
#1 Posted : 1/27/2022 5:22:06 PM

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Mindlusion already pointed out MeO needs to be as pure as possible to induce any crystalization. n-Hexane + optional drops of Ethyl Acetate might do great. Interestingly, when it oils out to a freebase cake (which still solidifies), it is completely orange even at full purity. Still, also DMT solutions turn yellowish, even if the crystals were white. Maybe a good thing - so people dont throw away their goodies by accident Laughing

Now I could check out this Molecule and it seems as long as it is completely pure it will always crystalize even with plain n-Hexane. Using Nephtha (C6-C7, 60-80 °C) was also tested ...

For the later one the solubility is 40 % higher (for actual values check the link further down). Not sure if this really is the job of the Heptane or caused by the simple addition of 10 K higher max. Temperature. Nevertheless this comes with a downside ...
Much more MeO-DMT dissolves, so it also drops much faster in max. Saturation, as both Solvents basically dissolve 0 % at Room Temperature (unlike DMT, where you need to get down to -20 °C to hit the same low solubility).
That's why the precipitation is too fast to induce crystallization at the beginning, but then also creating some beautiful crystals later on as a nice topping to your amorph orange freebase rock bottom.

For how much solvent to use, refer to this page. Still, using an extent is no Problem (unlike with Spice), as the Solvent holds basically 0 product back at Room Temperature.

As n-Hexane produces clean crystals, I would simply suggest to throw any amount of n-Hexane on your crude Material, given that it exceeds the minimum solvent amount calculated from the link above. Then just let it rest at RT, there is no more precipitation in the Fridge / Freezer (< 1 mg/ml solubility at RT). As you barely loose any material, you can simply throw in the next fresh Hexane to get to white crystals in 2 rounds of re-x.

Important: Dont blow on your Hexane-Surface! This will act like a rough forced nucleation source, making the material oil out on the surface and drip down once coagulated droplets get too heavy. It's so important as I could see constantly new droplets forming, even when just coughed 1x on top of it (no Covid promised), so Recrystalization needs to be restarted or you will have a mixture of orange balls inside of white crystals :/ So after carrying your hot mix over into another vessel for cooling down, just directly close it with a lid. Crystalization is over in less than 3 h.



Following you can see the process with both solvents.


 

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Brennendes Wasser
#2 Posted : 1/27/2022 5:23:29 PM

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I also wanted to make some stylo microscopy fotos. Sadly these crystals grew in a too high bottle, so the objective could not get down into focus.

So I had to grow them again in a small plate. I was sad first as they grew mascroscopically way less appealing ...

But in the end this was even way cooler, as the crystals only grew in small clusters all over the place, with random orientation.

Zooming into this revealed a multi-chromatic world full of crazy games of colors and geometry in the single-micron dimension.

You may argue that's where it got its bioactivity from Big grin Big grin Laughing

PS: I messed up the scale-bars for Picture #2 Left, #3 Left ... obviously it has to be exactly the same like #2 Right, #3 Right Rolling eyes


(Pictures taken with 250X - 1000X Lens.)


 
benzyme
#3 Posted : 1/27/2022 11:49:21 PM

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Brennendes Wasser wrote:
Interestingly, when it oils out to a freebase cake (which still solidifies), it is completely orange even at full purity. Still, also DMT solutions turn yellowish, even if the crystals were white. Maybe a good thing - so people dont throw away their goodies by accident


This has been a discussion I've had several times on the reddit subs, and the topic of many threads..

I elucidated a very plausible explanation that it is indicative of indole autooxidation, and occurs even with tryptamine itself (I've witnessed it isolating pure tryptamine). The source of oxidation (loss of electrons, which lack any discernible mass *hint hint*) is the pyrrole moiety, at the 2-3 positions.

For some strange reason, people believe a yellow/orange supersaturated solution of polymorphs means there must be fats...a misguided assumption at best.

I've also seen pure synthetic 5-MeO-DMT turn from clear to orange.

the only way to prevent coloration, is cold precipitation, purged with inert, heavier-than-air gas, like argon. A schlenk tube would be ideal.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Mindlusion
#4 Posted : 1/28/2022 4:00:36 AM

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benzyme wrote:
Brennendes Wasser wrote:
Interestingly, when it oils out to a freebase cake (which still solidifies), it is completely orange even at full purity. Still, also DMT solutions turn yellowish, even if the crystals were white. Maybe a good thing - so people dont throw away their goodies by accident


This has been a discussion I've had several times on the reddit subs, and the topic of many threads..

I elucidated a very plausible explanation that it is indicative of indole autooxidation, and occurs even with tryptamine itself (I've witnessed it isolating pure tryptamine). The source of oxidation (loss of electrons, which lack any discernible mass *hint hint*) is the pyrrole moiety, at the 2-3 positions.

For some strange reason, people believe a yellow/orange supersaturated solution of polymorphs means there must be fats...a misguided assumption at best.

I've also seen pure synthetic 5-MeO-DMT turn from clear to orange.

the only way to prevent coloration, is cold precipitation, purged with inert, heavier-than-air gas, like argon. A schlenk tube would be ideal.



I wish we could end this once and for all, the color from tryptamines is NOT and has NOTHING to do with fats and oils!

I have witnessed chromatographically pure DMT, 5-meo-DMT, and other tryptamines produce changing and unusually broad peaks in their 1H NMR spectra. Normally , with the tryptamines that produce these broad peaks, they often do not crystallize, either as the freebase or as their fumarate or HCl salts. Instead they form an amorphous goo, that can only be solidified into a dry foam when heated and pumped under high vac. With repeated crystallizations, (hexanes with a couple drops of ethyl acetate is indeed good for fb 5-meo-DMT) pure crystals can be obtained eventually. Colour is not always correlated though with the challenge in crystallization though, I have had this occur with totally colorless products as well I have investigated these broad peaks as a result of borane adducts, as a byproduct in the case with synthetic products, but that is a different story. The colour emerges with practically any small molecule with an indole backbone, oxidation at the C-2, C-3, indole is like a bucket overflowing with electrons, given enough time, thermodynamics takes place and these electrons will drain into whatever available sink, the oxidant, be it facilitated by oxygen or something else. Even in a glovebox, indoles will eventually discolor even among traces of oxygen given months or years sitting in a vial. This process is much faster especially with indoles in solution, the alkyl amine moiety in tryptamines only accelerates this, especially in free base form.
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benzyme
#5 Posted : 1/28/2022 4:04:42 AM

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seriously.

but for some weird reason, people reject scientific explanations, and still attribute coloration to fats without citing any evidence or explanation to support it. Just belief, like religious zealots. Willful ignorance.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Brennendes Wasser
#6 Posted : 1/28/2022 8:26:17 AM

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Similar to oils it's also a weird believe to often blame reddish material to N-Oxide. This compound will not even evade by just thermal treatment and later on be insoluble in Hexan anyways. The only possibility to get the N-Oxide in your product at more than analytical traces would be by intentional forcing it Confused
 
Mindlusion
#7 Posted : 1/28/2022 5:29:05 PM

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Brennendes Wasser wrote:
Similar to oils it's also a weird believe to often blame reddish material to N-Oxide. This compound will not even evade by just thermal treatment and later on be insoluble in Hexan anyways. The only possibility to get the N-Oxide in your product at more than analytical traces would be by intentional forcing it Confused



This is true. Another common misconception. N oxides, are trace impurities at best, but more importantly they are so different in properties compared to amines (n-oxides are not basic), that it is virtually impossible for them to end up in product after an acid base extraction work up. They are typically only seen in relevant concentrations when one intends it, like with the addition of hydrogen peroxide. But again this information is disregarded and instead people assume that n-oxides are a corporeal component, and instead of giving the chemical rational, citing that zinc can increase your dmt yield in old bark Confused Which is not wrong persay, but the error propagates when people take one fact and then blindly apply it to other circumstances and make assumptions, without thinking about first principles, and that's how it catches on.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
 
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