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DMT fumarate crystalisation and yield problem

Vularin

Vularin

Rising Star
Hiya peeps! :)

Im having a problem with making making Fumarate DMT. I have done lazy tek and freebase to fumarate tek (using 69ron tek, The FASA Method: A Summary - DMT Fumarate and Beyond - FASA/FASI/FASW - Welcome to the DMT-Nexus).

But somehow the yield seems to be off.


First freebase to fumarate:

I have noticed with this that after the crystals have formed i put them aside for a night (room temp), the next morning however they seem to have melted and schrunk alot. Also they become really hard. Yield has gone from 1000mg to about 400mg.


Second Lazy tek clean up:

When i solve, lazy tek fumarate (to get rid of the d-limo smell and taste) in warm 99% IPA and freeze solution for two days, im left with almost the same amount that recrystalises. However again when i drain the crystals and leave them to dry overnight, almost all the dmt fumarate has dissappeard and formed same like hard substance. Again it went from the original 5000 to 1000 mg just from drying.

-- stangly, the resulting product doesnt desolve in lab grade MEK


So anyone know what is happening here? I have used all the right measurment for the teks but i just dont get why i loose so much dmt.

Please help and thanks!
V
 
freebase to fumarate:

you say 'yield has gone from 1000mg to 400mg'.. When did you measure the 1000mg? The dmt cant have dissapeared anywhere.. Did you throw anything away?

Lazy tek clean up:

First question, which lazy tek clean up do you mean? got a link?

And again, when did you measure 5000mg, before recrystalizing? Did you throw the IPA from recrystalization away? How much IPA did you use for that amount of fumarates? Is it possible you used too much IPA and some of the fumarates is still dissolved in it? Maybe you should leave for longer than 3 days in the freezer. Is the freezer in the coldest setting? You could evap the IPA and see if there is anything left there.

As for the dmt fumarate becoming a 'hard like substance', well, as long as its fumarates, it doesnt really matter if its nice crystals or if it got harder, right?
 
A: freebase to fumarate:

tek used:
-Completely dissolve 1000 mg of freebase DMT in 50 ml of acetone.
-Completely dissolve 309 mg of fumaric acid in another batch of 50 ml of acetone.
-Mix for 1 minute and evaporate at room temperature to give DMT fumarate.

When i added the freebase dmt/acetone to the fumarate /acetone. crystals from and i let it set for a couple of hours. then i decanted the acetone and bunch of crystals were at the bottom. I let the remaining trace amount of acetone evap. Strangle enough the dmt crystals seemed alot less the next day....

Lazy tek clean up:

tek used to get fumarate:

BLAB - The Big Leisurely A/B - DMT-Nexus Wiki

wiki.dmt-nexus.me wiki.dmt-nexus.me

then the fumarate i got as result. i washed a couple times with cold IPA. but dlimo taste was still there (didnt loose alot of dmt fuma in this process) so i did warm IPA wash. I didnt measure this cause i dont have a tek to use for right volumes.

However after doing the warm IPA desolve and in the freezer (-15 C) for two days lots of crystal precipped. Decanting that produced alot of end product that looked very white and sparkly and was rather dry. Were it gets strange is that leaving it overnight to evap even more, the next day most of it was gone.

I can only imagine two problems, maybe the IPA was too hot or drying on a coffee filter ruined the yield..
 
Vularin said:
A: freebase to fumarate:

tek used:
-Completely dissolve 1000 mg of freebase DMT in 50 ml of acetone.
-Completely dissolve 309 mg of fumaric acid in another batch of 50 ml of acetone.
-Mix for 1 minute and evaporate at room temperature to give DMT fumarate.

When i added the freebase dmt/acetone to the fumarate /acetone. crystals from and i let it set for a couple of hours. then i decanted the acetone and bunch of crystals were at the bottom. I let the remaining trace amount of acetone evap. Strangle enough the dmt crystals seemed alot less the next day....
Click to expand...


The DMT didnt dissapear out of thin air, conservation of mass principle says your DMT must be there :D You must have 1309mg fumarate (or 1309mg 'something'). .. did you evap all the acetone and retrieve the product that was in it, appart from what precipitated out of the acetone when mixing the dmt/acetone and fumarate/acetone? When you say it 'seemed like less', are you talking about visually? Well, before things are dry, they have a different appearance then when dry, but that shouldnt matter.. As long as you have all your 1309mg there, they can look less or more for all you care, right? :D

Vularin said:
Lazy tek clean up:

tek used to get fumarate:

BLAB - The Big Leisurely A/B - DMT-Nexus Wiki

wiki.dmt-nexus.me wiki.dmt-nexus.me

then the fumarate i got as result. i washed a couple times with cold IPA. but dlimo taste was still there (didnt loose alot of dmt fuma in this process) so i did warm IPA wash. I didnt measure this cause i dont have a tek to use for right volumes.

However after doing the warm IPA desolve and in the freezer (-15 C) for two days lots of crystal precipped. Decanting that produced alot of end product that looked very white and sparkly and was rather dry. Were it gets strange is that leaving it overnight to evap even more, the next day most of it was gone.

I can only imagine two problems, maybe the IPA was too hot or drying on a coffee filter ruined the yield..
Click to expand...

Again, your dmt fumarate wont have dissapeared anywhere, it must be somewhere. Here's what I can imagine:

Possibility 1: it maybe 'seemed' like plenty was precipitated but a lot of it was still in the IPA, so leaving for longer in the freezer and/or using less IPA to dissolve it all might be a better idea for next time. Evap all your IPA and see if there is anything in it.

Possibility 2: Your IPA picked up water from the air/freezer before or during freeze precip, so some of your DMT stayed dissolved in the wet IPA. Evap all your IPA and see if there's anything in it.

Possibility 3: As your IPA warmed up and evapped, it dissolved some of your fumarate, maybe also because it trapped some water from the air. So it melted through your coffee filter. Maybe your coffee filter has been infused with dmt fumarate, and/or maybe the container/funnel that is under the filter has some of your dmt fumarate. Wash the filter/container with a bit of warm water and evap that, to see if you retrieve anything. Next time to dry, just leave it standing in a dish/hard-bottom-container without using a coffee filter so that any dissolved fumarate will remain where it is, so you can scrape later
 
I think i know what the problem could be.

Seeing that the Fumarate seems to shrink when drying and ends up in the filter, causes me to believe that there is still lots of oxide or jungle present.
This explains it cause at room temp the oxide/jungle becomes goo when the solvent evaps.

See my other post here: possible MEK to clean DMT fumarate - FASA/FASI/FASW - Welcome to the DMT-Nexus

So im think after doing a FASA conversion or IPA wash, before completly drying it, do a MEK wash!!

V
 
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