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Pure DMT Fumarate from freebase DMT Options
 
Infundibulum
#81 Posted : 8/26/2008 9:40:47 PM

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That is true, salt form is very dry and easy to handle. Even jungle spice can be salted out in which case it is a nice solid in contrast to the honey-like texture it freebase equivalent. (should be nice to snort it, something SWIM hasn't done yet!)

And of course, it is a very nice way for getting clean freebase from it, since one can dissolve the salt in water, basify and pull with xylene. (SWIM says xylene because it can get the most of alkaloids out of the basified solution with the least amount of solvent used. DCM should work wonders here SWIM guesses..)

SWIM is supposed to be working on some ideas to get the freebase from the salt in fewer steps but he's soooo lazy lately....


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 

STS is a community for people interested in growing, preserving and researching botanical species, particularly those with remarkable therapeutic and/or psychoactive properties.
 
amor_fati
#82 Posted : 8/27/2008 6:23:26 AM

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Seems like this salting method could easily put all considerations about evaping xylene to rest. It's certainly got its uses, and if there's no evap involved, the fumes are a minor nuisance. Not to mention that SWIM'll finally have reasonable access to jungle-spice.

Some quick questions though, partially off-topic: SWIM's likely got some jungle-spice (from final extractions) in his xylene mixed in with a good amount of presumably pure spice (from the pipe-washing), and so SWIM'd imagine it'd be a good idea to keep this separate from a regular stash of spice? SWIM's concern is the difference in psychoactivity between the two. He should probably refrain from using the same xylene for both purposes anyway, but SWIM has a feeling the resulting product's going to have a pretty gritty character, regardless. Also, are there noticeable differences in hue or smell or between the jungle fumarate and the standard?

Quote:
In a SWIM's pilot experiment fumarate alkaloids were dissolved in the minimum amount of water, basified and then let it sit at room temperature. This milky solution got clear after 2 days and SWIM could observe wee shiny crystals sitting on the bottom and the sides of the tube trying to protect themselves from the hostile aqueous environment...How cute!


SWIM was also wondering how solid or rocky that precipitate turned out to be. Would one have to recrystallize in an NPS? Two days is a while though, perhaps there's a better polar solvent that could be basified and used in place of water (probably what you're considering anyway)? Otherwise, SWIM would probably pull with an NPS right off the bat, since freebase sediment in aqueous seems like a pain anyway.
 
Infundibulum
#83 Posted : 8/27/2008 12:04:38 PM

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amor_fati wrote:
I was also wondering how solid or rocky that precipitate turned out to be. Would one have to recrystallize in an NPS? Two days is a while though, perhaps there's a better polar solvent that could be basified and used in place of water (probably what you're considering anyway)? Otherwise, I would probably pull with an NPS right off the bat, since freebase sediment in aqueous seems like a pain anyway.


SWIM is now repeating the freebase crystallisation inside the basified solution thing, this time taking pictures of the process. From his last experiment, the crystals seemed to be transparent with waxy feeling (they were sticking to the sides of the polypropylene tube as well as the bottom) and they could not be agitated. SWIM remembers shaking the basic solution to detach them from the sides (hoping that they will eventually fall on the bottom) but they didn't detach!

This was not much unexpected, if one imagines the freebase to have a waxy texture and to feel uncomfortable inside the aqueous solution...

But enough said about this one-off-freehanded-fool-around experiment! Unless this is not consistently repeated and properly documented by SWIM there's not much reason to talk about it!

And of course, as you mentioned the alternative is always the good ol' NP solvent route!

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Viracocha
#84 Posted : 8/27/2008 12:36:24 PM

..still lc..


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seems like the dmt.f fairy visited
ie, crystals no more

dang hygroscopic silliness
at least that confirms what they are, even a freebase wouldn't do that
 
Infundibulum
#85 Posted : 8/27/2008 12:53:06 PM

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Try sticking them in the oven; SWIM did that at 70 Celsius for I cannot remember, maybe half to 1 hour. They should quickly lose their moisture and become very solid!

dmt-fumarate is in fact quite hygroscopic but not as much as the other salts. At least it can be dried out. SWIM lately did some dmt-citrate, now this is some goo, it behaved exactly like honey.

(SWIM in the beginning tried a desiccator filled with silica gel to absorb the moisture from the dmt-fumarate. Eventually he found that oven works much much better and much much faster.)


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Viracocha
#86 Posted : 8/28/2008 7:27:11 AM

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Ok, complete success. Here's what was done:

Initially, no precipitate was seen, although it may have been too dilute to see.
Those crystals that formed I mentioned above were most definitely dmt.fumarate. Anyway, the entirety of the acetone (initially containing 500mg of dmt freebase and 500mg of fumaric acid) was allowed to evaporate.

There was an obvious mixture of components after evap. They were scraped up and found to be noticably wet (even though 50mL of the acetone does evaporate to dryness and there was no scent of acetone remaining).

The crystals were placed in a jar, covered with 100mL of fresh acetone and agitated in attempt to remove any excess fumaric acid. The solution was let to sit for an hour which allowed all the precipitate to fall to the bottom. The acetone was poured off being careful not to let any of the precipitate come out. The precipitate was allowed to 'dry' (evaporate the rest of the acetone until no scent remains). This took about half an hour. The powder was scraped and found to be completely dry, weighing in at 648mg !!!! That's bullshit accuracy if you ask me, but I'm not complaining. The powder is visibly a single component, water soluble, and extremely tangy on taste.

Ronue.. dude Wink


Fyi,
By calculation, the amount of fumaric acid needed is 0.31 x the amount of dmt freebase used. For good measure, a 0.4 is used:

Future (and in progress) experiment:

-Dissolve 500mg of dmt freebase in 10mL of acetone (2mL/100mg)
-Dissolve 200mg of fumaric acid in 50mL of acetone (25mL/100mg)
-Add the the fumaric acid soln slowly(ish) to the dmt soln

for curiousity, pH was measured and found to be just slightly acidic - good!

after combining the two solution, a single solution which looked like milk was formed (dmt.fumarate precipitated). Within 15 minutes it can be seen that glass shard type crystals are forming. The jar is allowed to sit (covered) overnight to afford the crystallistaion ample time to complete.

-once crystallisation is complete, the acetone is poured off and the crystals are allowed to dry
-once no scent of acetone remains, the crystals are scraped up, powdered and added to 25mL of fresh acetone. Stirred well, allowed to settle for an hour or so, and then the acetone poured off, the crystals dried, scraped up and weighed. They should weight approx 1.3 times the weight of the dmt freebase used
 
drainlife20
#87 Posted : 9/1/2008 1:05:03 AM

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I think I asked this already, but has anybody had experience with using the fumarate? I've read much about the process, and it definitely seems to be very good for storage, but what about using it as is? Anyone know anybody with experience? Was an MAOI snorted as well? Etc?
Thanks for reading my dream diary! I hope you found it interesting! LMBO!
 
Infundibulum
#88 Posted : 9/1/2008 1:51:33 AM

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Hey drainlife,

50mg dmt-fumarate snorted just gave body load

150mg snorted gave a ~45min trip, fairly mild, very dreamy state, OEVs became apparent 3 min after snorting. CEVs contained musky tones, not bright colours but they had the typical tryptamine character. SWIM felt the presence of entities (or guides?). Overall, very manageable and worth trying.

It was not very manageable in the nose, 150mg is already a big amount, it burned a bit but nothing really too uncomfortable!


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Infundibulum
#89 Posted : 9/1/2008 1:54:05 AM

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OK, this is the experiment describing the conversion of dmt fumarate to freebase without using any NP solvents, it just relies on the crystallisation of the freebase inside a basified solution.

Enjoy!


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
amor_fati
#90 Posted : 9/2/2008 6:27:06 AM

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Just seeing the fumarate in the vial with no crumbs stuck to the sides was absolutely heart-warming.

Is there any significant loss with this method? Would you recommend mixing the filtered solution with the NPS before dissolving the freebase?
 
Infundibulum
#91 Posted : 9/2/2008 3:20:06 PM

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SWIM doesn't know...He just assumes that after 3 days all freebase must have crystallised. Still need to retrieve it and weight it. If it's less that ~70m then some of it still remains in the basic solution.


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Viracocha
#92 Posted : 9/3/2008 10:25:48 AM

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500mg salted came to 644mg on one occassion
on the other it was 648mg

Both times the they were washed with acetone to remove any residual fumaric acid

Basically, it comes down to how efficiently you can scrape up the crystal


I suspect crystallisation is finished within a matter of hours, if not minutes. But i could be wrong Very happy
 
amor_fati
#93 Posted : 9/3/2008 5:31:38 PM

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Incredible.... SWIM started out with less than a tenth of this vial left of freebase, and a big jar of xylene (containing jungle-spice and resin). This vial held nearly 6g of freebase from my last extraction before most of it was smoked. Now, SWIM's filled it again thanks to the contributions made on this thread--though this time with fumarate.

SWIM played around with it in the salting process to get a feel for it and unfortunately lost a good amount to the sides of several containers. SWIM was slightly disheartened until SWIM realized that he could simply wash it out with water and save the water for when he wishes to make freebase again.

SWIM's a little worried to wash with acetone, though supposes he had better if he's to administer it through insuffulation (w/ harmala).

This will be extremely handy for my next extraction. Nice work!
amor_fati attached the following image(s):
P1040430.JPG (65kb) downloaded 499 time(s).
 
Viracocha
#94 Posted : 9/4/2008 12:10:42 AM

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lol nice background man Laughing

Why worry about washing it with acetone?
It's basically the same deal as the first time

Anyway, excess fumaric acid isn't too bad
 
amor_fati
#95 Posted : 9/4/2008 4:57:20 AM

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Oh yes, but it's just so dry and pretty!

SWIM did a couple rails and is pretty sure he should wash it, because it burned pretty bad. It wasn't nearly as bad as freebase, though.
 
Viracocha
#96 Posted : 9/4/2008 10:26:45 AM

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Argh, jesus f'n christ
I snorting 70mg of freebase once.. never again, ever, whoa, bad

The fumarate is a pleasure

I was thinking about this,
eh, too much to write now, shortly you'll see what i'm talking about
 
amor_fati
#97 Posted : 9/11/2008 2:22:31 PM

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Since fumarate salting relies so heavily on acetone, SWIM thought he might share this method of making anhydrous acetone:

Quote:
You can easily turn hardware store acetone into anhydrous acetone with the simple process I've outlined below. To do this, you'll need to go to Home Depot or Lowes and get the following items: a 1 liter can of acetone, a bag of epsom salts, and a bottle of 31% muriatic acid.

Now, heat some epsom salts on an aluminum foil covered baking sheet in the oven for 2 hours at 400 degrees F. After 2 hours of heating, the epsom salts have now been turned into anhydrous magnesium sulphate. Crazy huh?

Now, take 10-20 grams of your greyish ash looking anhydrous magnesium sulphate and pour it directly into your can of hardware store acetone. Now, shake the can vigorously for a few minutes to circulate the magnesium sulphate and then let it settle for 24 hours. The magnesium sulphate will absorb all of the water and/or alcohol from the hardware store acetone and sink it to the bottom of the can where it shall remain forever.

Therefore from now on, never pour from the can, instead use a glass eye dropper or glass pipette (glass straw) to reach down inside of the can to extract however much anhydrous acetone you'll be requiring. Always stay away from the bottom of the can. Once the can get's about half way down, discard and repeat the process with a fresh can of acetone. Always use glass hardware when using acetone. Acetone will melt plastic.

from bluelight
 
kemist
#98 Posted : 9/13/2008 7:44:51 AM

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69ron wrote:
Pure DMT fumarate from freebase DMT.

To make pure DMT fumarate from freebase DMT the following procedure from SWIM’s notes works great

Quote:
1) Dissolve 100 mg of DMT in 4 ml of warm 91% isopropyl alcohol (about 40 C). NOTE: substitutes that also work include 95% ethanol, 95 % isopropyl alcohol. Hoever 99% does not work. There must be at least 5% water or the fumaric acid in the next step fails to dissolve completely.
2) Add 100 mg of fumaric acid. NOTE: this is excess fumaric acid. We actually only need 31 mg in theory, but we use 100 just to make sure.
3) Evaporate the solution at no hotter than 140 C (DMT fumarate melts at 152 C). NOTE: putting the liquid in a 10 ml beaker on a hotplate set to 100 C with a fan blowing over the liquid works great.
4) When completely dry, we add 10 ml of methyl ethyl ketone and mix. The excess fumaric acid quickly falls to the bottom of the methyl ethyl ketone because it’s insoluble in it.
5) Filter the methyl ethyl ketone to remove the excess fumaric acid.
6) Evaporate the solution at no hotter than 140 C (DMT fumarate melts at 152 C) to give pure DMT fumarate crystals.

Freebase DMT has a molecular weight of about 188.269. Fumaric acid has a molecular weight of 116.07. DMT fumarate has a molecular weight of about 492.608 (DMT + fumaric acid + DMT). It is 76% as potent as freebase DMT, so you’ll need 31% more to achieve the same effectiveness. This means a 20 mg dose of freebase DMT is equivalent to 26 mg of DMT fumarate (requiring 31% more).

DMT fumarate is more water soluble, more stable, has a longer shelf life, is much easier to crystallize, has a higher melting point, is less waxy, and easier to form into a powder than freebase DMT. Because of these characteristics DMT fumarate is much preferred over freebase DMT. Freebase DMT has no benefits other than the fact that it is easily vaporized.

EDIT: DON'T TRY THIS TECH!!! There's an error in it. SWIM is looking into this and will fix this tech. Until then DON'T TRY IT. It doesn't work as stated. SWIM thinks maybe the acid was MISLABELED IN HIS LAB.


[[[ 4) When completely dry, we add 10 ml of methyl ethyl ketone and mix. The excess fumaric acid quickly falls to the bottom of the methyl ethyl ketone because it’s insoluble in it. ]]]

HI 69RON, ILPT would like to ask SWIM if he can use in this charming tek blend of MEK and Metyl Isobutyl ketone instead of pure MEK? ILPT found this clean blend easily available as the cellulose thinner.
As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 
69ron
#99 Posted : 9/13/2008 8:04:56 AM

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That tech is flawed. It doesn’t work as stated. Something in SWIM’s notes were messed up.

One SWIM said the MEK part is backwards in that tech and that the DMT Fumarate is insoluble in the MEK and the DMT Fumarate gets filtered out and the excess fumaric acid stays in the MEK.

SWIM's lab is under construction right now so he hasn't found the problem yet. Once his lab is back to normal he’ll fix that tech.


Methyl isobutyl ketone (MIBK) is a GREAT SOLVENT! It's better than MEK because it’s only 2% water soluble. MEK is 29% water soluble. It should work as a substitute for MEK but only in some cases.

MEK has an XLogP of 0.4

Acetone has an XLogP of 0.2

MIBK has an XLogP of 1.5, that’s the same as DCM. That means that MIBK can be used as a DCM substitute for many extractions requiring DCM. I think both fumaric acid and DMT fumarate are probably not soluble in MIBK, but SWIM never tested it.

Give it a try. Just make sure to save everything just in case it doesn’t work. At worst, it will do nothing and so you can evaporate everything to recover your stuff.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
kemist
#100 Posted : 9/15/2008 8:07:33 PM

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Uno Excellento Maestro 69Ron. ILPT will go for that blend and whilst ILPT waiting for DCM delivery he try pull some dmt from amonium basified acetic extract of MHBR. Wauu Smile
As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 
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