I’ve got some 5-MeO-DMT freebase, but I’d like to try it nasally, which means I need it in a salt form. I’ve tried working with succinic acid and acetone, as well as with the freebase and acetone, to make a salt, but I haven’t had much success so far. I’m wondering if anyone here might have some advice on how to get this to work properly.
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Trouble Making a 5-MeO-DMT Salt – Need Some Guidance
- Thread starter FelixFox
- Start date
Hi, welcome!
First of all, try telling us exactly what you've done so far, what your plan was, and how you concluded that it didn't work. Include as much detail as you can.
If you look through the posts of @Jan e Kharabat you should find some salient information, too.
Ok, so I encountered a procedure on Reddit (see attachment) and, after consulting with a chemist, attempted the conversion of synthetic 5-MeO-DMT utilizing succinic acid powder and acetone.
Initially, 1 g of 5-MeO-DMT freebase and 550 mg of succinic acid were separately dissolved in acetone—both requiring extended time to achieve solubility. The solutions were then combined on a flat surface to facilitate subsequent crystal recovery. Post-evaporation of the acetone, no crystalline salt formed; instead, a viscous, brownish paste was observed (see attachment).
In a subsequent attempt, the paste was redissolved in acetone, followed by the gradual addition of an acetone solution containing an additional 300 mg of succinic acid. This process led to partial precipitation, while a portion remained as a brownish paste. After drying, the precipitate appeared as a reddish-brown crystalline powder.
Due to concerns that the product may represent an incomplete salt formation—potentially a salt-freebase mixture with mucosal irritant properties—I have refrained from testing. Additionally, the reddish-brown coloration raises concerns, as a white crystalline form was anticipated.
I seek insights on potential procedural errors and recommendations for further refinement. Thank you for your expertise.
Initially, 1 g of 5-MeO-DMT freebase and 550 mg of succinic acid were separately dissolved in acetone—both requiring extended time to achieve solubility. The solutions were then combined on a flat surface to facilitate subsequent crystal recovery. Post-evaporation of the acetone, no crystalline salt formed; instead, a viscous, brownish paste was observed (see attachment).
In a subsequent attempt, the paste was redissolved in acetone, followed by the gradual addition of an acetone solution containing an additional 300 mg of succinic acid. This process led to partial precipitation, while a portion remained as a brownish paste. After drying, the precipitate appeared as a reddish-brown crystalline powder.
Due to concerns that the product may represent an incomplete salt formation—potentially a salt-freebase mixture with mucosal irritant properties—I have refrained from testing. Additionally, the reddish-brown coloration raises concerns, as a white crystalline form was anticipated.
I seek insights on potential procedural errors and recommendations for further refinement. Thank you for your expertise.
Oiling out of tryptamines isn't at all uncommon, especially from more concentrated solutions.
Your approach also seems to have failed to acknowledge the general principle of the analogous FASA precipitation, although I can't off the top of my head say that 5-MeO-DMT succinates would be similarly insoluble in anhydrous acetone like 2:1DMT fumarate is. Suffice to say, it may have been more prudent to have had your tryptamine/acetone solution in a test tube and added the SASA (i.e. succinic acid saturated acetone) dropwise while observing for formation of a precipitate, as per FASA.
This brings up a further point - using a large surface area for the preparation greatly increases the rate at which acetone absorbs atmospheric moisture and this consequently leads to the oily crust which you were left with. Part of the mechanism there is that the water greatly increases the solubility of 5-MeO-DMT succinate in the system, leading to a highly concentrated solution which is intrinsically prone to amorphous solidification.
At least when working with DMT fumarate, it has proven to be important to make a substantial effort to ensure ones acetone contains as little water as possible. It would be a matter of checking out the solubility data for 5-MeO-DMT succinate or the corresponding hydrogensuccinate (should that data even exist) and carrying out some careful solubility experiments if necessary.
You could try recrystallising your product from boiling 99+% isopropanol. This would also help clean up any inconsisencies in stoichiometry, i.e. dissolve an excess of either of the components. But, like I've said, there's no guarantee that the salt you've been attempting to prepare will have a similar solubility profile to that of DMT fumarate.
Remember not to discard anything without first having accounted for losses!
pubchem.ncbi.nlm.nih.gov
pubchem.ncbi.nlm.nih.gov
→CAS 2568048-63-3
Cayman Chemical lists the following solubility properties:
DMF: 11 mg/ml
DMSO: 20 mg/ml
Ethanol: Slightly soluble
PBS* (pH 7.2): 5 mg/ml [this latter one being questionable]
[*PBS = phosphate-buffered saline]
Therefore, you may also be able to recrystallise from anhydrous ethanol.
(Note that recrystallisation does not involve the complete evaporation of the solvent!)
Your approach also seems to have failed to acknowledge the general principle of the analogous FASA precipitation, although I can't off the top of my head say that 5-MeO-DMT succinates would be similarly insoluble in anhydrous acetone like 2:1DMT fumarate is. Suffice to say, it may have been more prudent to have had your tryptamine/acetone solution in a test tube and added the SASA (i.e. succinic acid saturated acetone) dropwise while observing for formation of a precipitate, as per FASA.
This brings up a further point - using a large surface area for the preparation greatly increases the rate at which acetone absorbs atmospheric moisture and this consequently leads to the oily crust which you were left with. Part of the mechanism there is that the water greatly increases the solubility of 5-MeO-DMT succinate in the system, leading to a highly concentrated solution which is intrinsically prone to amorphous solidification.
At least when working with DMT fumarate, it has proven to be important to make a substantial effort to ensure ones acetone contains as little water as possible. It would be a matter of checking out the solubility data for 5-MeO-DMT succinate or the corresponding hydrogensuccinate (should that data even exist) and carrying out some careful solubility experiments if necessary.
You could try recrystallising your product from boiling 99+% isopropanol. This would also help clean up any inconsisencies in stoichiometry, i.e. dissolve an excess of either of the components. But, like I've said, there's no guarantee that the salt you've been attempting to prepare will have a similar solubility profile to that of DMT fumarate.
Remember not to discard anything without first having accounted for losses!
5-methoxy DMT (fumarate)
5-methoxy DMT (fumarate) | C17H22N2O5 | CID 166791753 - structure, chemical names, physical and chemical properties, classification, patents, literature, biological activities, safety/hazards/toxicity information, supplier lists, and more.
pubchem.ncbi.nlm.nih.gov
Mebufotenin succinate
Mebufotenin succinate | C17H24N2O5 | CID 164886348 - structure, chemical names, physical and chemical properties, classification, patents, literature, biological activities, safety/hazards/toxicity information, supplier lists, and more.
pubchem.ncbi.nlm.nih.gov
Cayman Chemical lists the following solubility properties:
DMF: 11 mg/ml
DMSO: 20 mg/ml
Ethanol: Slightly soluble
PBS* (pH 7.2): 5 mg/ml [this latter one being questionable]
[*PBS = phosphate-buffered saline]
Therefore, you may also be able to recrystallise from anhydrous ethanol.
(Note that recrystallisation does not involve the complete evaporation of the solvent!)
aizoaceous
Titanium Teammate
Ott reports intranasal and sublingual use of 5-MeO-DMT freebase, so I guess a salt isn't strictly required. I've never tried that myself. I'd guess the salt would at least be less irritating.
5-MeO-DMT salts have a reputation as hard to crystallize, and that may explain your failure. The oxalate is reportedly easiest, and I succeeded with that. I'd guess that would also be irritating though. I guess that reddit procedure chose the 1:1 succinate based on the Usona Institute's paper, which does say it precipitates from acetone (and gives lots of solubilities and other properties in the supporting information; they indeed suggest hot ethanol for crystallization). I tried their methods, but all my attempts failed. That might have been residual water like @Transform says, since my extract wasn't dried under vacuum and I worked in open air vs. their big rotovap. It might also have been the different impurity profile of my natural product vs. their synthetic. Beckley Psytech is running trials with the benzoate, which I haven't tried.
I'm not sure there's actually any need to crystallize, though? I've consumed mebufotenin-dominant Phalaris extracts intranasally and sublingually in liquid form, just by dissolving in water and citric acid to pH ~ 5. I don't think there's much history of such use, but it seems relatively safe to me (considering the tryptamines alone; other constituents of the crude plant alkaloids will at least temporarily impair your sense of smell, so purification is advised).
Note the general danger of this drug. Many serious overdoses are reported, including at least one death.
5-MeO-DMT salts have a reputation as hard to crystallize, and that may explain your failure. The oxalate is reportedly easiest, and I succeeded with that. I'd guess that would also be irritating though. I guess that reddit procedure chose the 1:1 succinate based on the Usona Institute's paper, which does say it precipitates from acetone (and gives lots of solubilities and other properties in the supporting information; they indeed suggest hot ethanol for crystallization). I tried their methods, but all my attempts failed. That might have been residual water like @Transform says, since my extract wasn't dried under vacuum and I worked in open air vs. their big rotovap. It might also have been the different impurity profile of my natural product vs. their synthetic. Beckley Psytech is running trials with the benzoate, which I haven't tried.
I'm not sure there's actually any need to crystallize, though? I've consumed mebufotenin-dominant Phalaris extracts intranasally and sublingually in liquid form, just by dissolving in water and citric acid to pH ~ 5. I don't think there's much history of such use, but it seems relatively safe to me (considering the tryptamines alone; other constituents of the crude plant alkaloids will at least temporarily impair your sense of smell, so purification is advised).
Note the general danger of this drug. Many serious overdoses are reported, including at least one death.
Ah, thanks! That Usona paper:
It's been mentioned on the forum before, now that you come to mention it, and I've no idea why it failed to come up in any of my searches - despite it being stickied in this very forum
forum.dmt-nexus.me
deserves to be in our science papers section
It's been mentioned on the forum before, now that you come to mention it, and I've no idea why it failed to come up in any of my searches - despite it being stickied in this very forum
Synthesis and Characterization of 5-MeO-DMT Succinate for Clinical Use
To support clinical use, a multigram-scale process has been developed to provide 5-MeO-DMT, a psychedelic natural product found in the parotid gland secretions of the toad, Incilius alvarius. Several synthetic routes were initially explored, and the selected process featured an optimized Fischer...
forum.dmt-nexus.me
Thanks for sharing your experience, that’s really helpful context.
I’ve been wondering about the intranasal route with 5-MeO-DMT freebase myself. Do you (or anyone else here) have any experience with it, and if so, what kind of dose tends to be used? I was also thinking about whether it could be dissolved in saline and administered via a nasal spray.
In my case, I already have this product now that I can’t fully identify – it might be a mix of succinate and freebase (see attachment). How would you proceed in a situation like that? Would it even make sense to try it intranasally, and what would be a cautious starting dose?
For context: I’m quite experienced with vaporizing 5-MeO-DMT – I do it regularly, use it therapeutically, and I feel very familiar with its effects. What attracts me to the nasal route is the potential for a longer, smoother onset and comedown compared to vaping.
Since you've prepared your material by evaporation of a solution containing known amounts, you should be able to calculate the percentage of freebase relative to the total mixture. For a given mass, m, of the salt, the equivalent amount of freebase will be
m*b/(a+b),
where 'b' is the amount of freebase and 'a' the amount of acid respectively used in the original acetone solutions.
So, say you weigh out 10mg of the material pictured, with the figures you've given it should contain
10*1/(1+0.55) = 10/1.55 =6.45mg
of 5-MeO-DMT.
You may want to check the molar ratios of the two components, as snorting excess acid could be uncomfortable.
m*b/(a+b),
where 'b' is the amount of freebase and 'a' the amount of acid respectively used in the original acetone solutions.
So, say you weigh out 10mg of the material pictured, with the figures you've given it should contain
10*1/(1+0.55) = 10/1.55 =6.45mg
of 5-MeO-DMT.
You may want to check the molar ratios of the two components, as snorting excess acid could be uncomfortable.
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