Fumarate - crystals forming then disappearing?

[Shattered_Symmetry]

Hi guys,

swim has just tried to convert his freebase dmt to fumarate via this tek. As the acetone began to evaporate nice looking long needle like crystals formed while there was still a small amount of acetone remaining.

Upon checking the dish later swim discovered that the crystals have disappeared and there is only liquid!!!! Could anyone tell me if this is indicant of something gone wrong?

 

[The Day Tripper]

I've never had crystals form then disappear when evaporating acetone with fb dmt in it. However, every time i have done this, its always came out as an oil that can be manually crystallized by scraping and working the oil. Eventually it clumps up to amorphous waxy clumps. I think if you want xtyals, its best to use a solvent dmt fb is less soluble in, (not acetone), and let it evap slowly. Alternatively, perhaps dissolving your oil/white waxy fb in a small amount of acetone, then slowly adding some water could cause it to precipitate nice crystals. Never tried that though, but i would like to sometime.

I just don't see crystals happening with tone, due to it being a good solvent for DMT, and evaporating rather quickly.

 

[Shattered_Symmetry]

My theory of what is happening is that the anhydrous acetone has absorbed water from the air during evap, this has lead to the dmt fumarate crystalising and then as water is absorbed by the acetone it has dissolved into the water as dmt fumarate is of course water soluble, the tek calls for the acetone to be drained off the top of the crystals when they form but i thought i would evap to ensure no product was lost. If my theory is correct then that is y u dont wait for the bloody evap!

At present there is a translucent brown oily substance in the evap dish which does not smell at all of acetone. it tastes bitter/sour, can anyone say what dmt fumarate tastes/smells like? my dish smells nothing like fb dmt.....

I would imagine it could only be absorbed water or some fucking impurity from bunk acetone or one of the other reagants

STRESS!!!

if anyone has any input on what is happening or how i might rescue my precious spice i would REALLY appreciate it!

Interesting that it comes out as an oil with fb dmt, i dont think fb is water soluble is it?

Also tripper, when you say "working the oil to manually crystalise" what do you mean?

 

[Infundibulum]

My theory of what is happening is that the anhydrous acetone has absorbed water from the air during evap, this has lead to the dmt fumarate crystalising and then as water is absorbed by the acetone it has dissolved into the water as dmt fumarate is of course water soluble,

this is exactly what has happened here. Just put this thing in the oven at 50 C for some time and this will dry off any water residues leaving behind crystalline goodies.

the tek calls for the acetone to be drained off the top of the crystals when they form but i thought i would evap to ensure no product was lost.

You should had drained off the acetone and keep the precipitates. What you have now is dmt fumarate PLUS any unreacted fumaric acid that remained in the acetone. By draining off the acetone you basically remove any unreacted fumaric acid leaving only dmt fumarate. Now your dmt fumarate is tainted with fumaric acid, hence it tastes bitter (the dmt fumarate portion) and sour (the fumaric acid portion)

In order to resolve this issue, wash your crystals (after drying them in the oven) with a good amount of acetone (same or more acetone as you used in the beginning of the tek)

 

[Shattered_Symmetry]

Thank you Infundiblum, I have dryed the residue by scraping it into a pool and smearing it across the dish then scraping it up again and repeating. I have found this to be efficacious in drying sticky residues. If the fumarate is to be administered orally via gel cap is there any point in risking loss of product through an acetone wash?

Edit: also the pre-wash yield from 2g fb was 2.36g of white/brown solids.

 

[The Day Tripper]

:lol: I totally thought you were talking about freebase.

Oh well, at least someone helped you figure it out.

As for working the oil to crystallize, for me, when i evap an amount of fasw, i usually do so under heat and it goes rather quickly. This is for fumerates btw, not freebase (which also comes out as an oil due to fast evaps). By evaping the water quickly you are left with an amorphous gooey yellowish oil. Scraping this oil up, and spreading it out again, doing so a few times, causes it to harden up and dry out/crystallize. After lots of scraping, its almost white, and i then proceed to finely powder it using a shot glass as a rolling pin to crush it in the pyrex evap dish. This happens no matter how pure/impure the fumarates are, but if i let it dry out slowly using little to no heat, crystals will form.

Fumarates are extremely soluble in hot water, so i think its all remaining soluble until the very end, and not crystallizing until almost all the water is gone. Since this happens so fast, (the transition from soluble in the water, to dry) theres no time for crystals to form.

Doing this ^ with freebase leaves you slightly waxy clumps of amorphous DMT. Definitely not crystals.