Converting DMT Freebase > DMT Fumarate (using FASI)

[Levanah]

Hi guys,

took following quote from this thread:

Here’s the quick tech:

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

Is it possible to do same with IPA to quickly and easy convert DMT Freebase to DMT Fumarate?

Thanks!

 

[DreaMTripper]

Sure is.

 

[Levanah]

Perfect, thanks DreamTripper! :thumb_up:

 

[Levanah]

Ok I finally did it. Exept the evap step.

Here's how it went:

1) Completely dissolved 1000 mg of freebase DMT in 50 ml of IPA.
2) Completely dissolved 309 mg of fumaric acid in another batch of 50 ml of IPA.
3) Mixed and shaked the two solutions for 1 minute

My question is: I was expecting that the combined Fumarate/DMT solution would get milky (=seeing DMT fumarate crash out)

-> Instead: The solution is still clear
-> Did these steps even in fridge-cold temperature where DMT Fumarate should not be soluble in IPA

<=> Has the convertion still worked properly and should I evap now to get DMT Fumarate?

Thanks! :thumb_up: Soon my sublingual ticture will be ready.

 

[Nereus]

Ok I finally did it. Exept the evap step.

Here's how it went:

1) Completely dissolved 1000 mg of freebase DMT in 50 ml of IPA.
2) Completely dissolved 309 mg of fumaric acid in another batch of 50 ml of IPA.
3) Mixed and shaked the two solutions for 1 minute

My question is: I was expecting that the combined Fumarate/DMT solution would get milky (=seeing DMT fumarate crash out)

-> Instead: The solution is still clear
-> Did these steps even in fridge-cold temperature where DMT Fumarate should not be soluble in IPA

<=> Has the convertion still worked properly and should I evap now to get DMT Fumarate?

Thanks! :thumb_up: Soon my sublingual ticture will be ready.

Yes. Sometimes it takes even up to 12 hrs for the reaction/precipitation to occur. Be patient and you will get nice results. Ime it does not have to stay in the fridge also, the anhydrous alcohol could absorb humidity from there...speaking of which, was your IPA dry?

Also for higher purity do not evap. While fumaric acid is soluble in IPA, DMT fumarate crystals are insoluble, thus they will crash out regardless of the temp being RT or cold.

Edit: Forgot to mention that clouding reactions only occur when doing FASA/FASI etc on extraction solvents like limo, xylene and so on.

For the conversion tek which uses IPA I have never actually encountered the clouding.

 

[Levanah]

Thanks for help and infos Nereus!

After putting the solution in the freezer for 15minutes it finally got cloudy. Then I evapped the IPA and within 2 hours I got the finest, fluffiest fumarate crystals that I have ever seen. I highly assume that they are fumarates, because I dissolved a tiny bit of it in water without residue.

Sometimes it takes even up to 12 hrs for the reaction/precipitation to occur. Be patient and you will get nice results.

In my understanding reaction and precipitation are two different things. The base-fumarate reaction itself might only take one minute rigorously shaking - if I am right?. Yes my IPA was 99,99%.

As my fumarate-acid / dmt-freebase ratio was precisely weighted, I assume there can't be a higher purity. There could be maximal 10mg fumarate-acid excess in the end which won't hurt in my case as everything will end up anyway in a glycerine-water ticture for sublingual/oral consumption.

Will let it the fluffy white dry some more, then dissolve it - if everything will dissolve without a problem in water, then the freebase-fumarate conversion worked out perfectly.

Here are some pictures:

 

[Nereus]

Well, I think it is more a case of preference rather than correctitude.In theory and also in regards to my advise to precip over evap, the idea was that any soluble impurities (or excess f.acid) present in the used starting material would remain suspended in soln, and decanting that off of the fully precipitated crystals would only result in a higher purity for the alks. Also this step would exclude the use of a fan (which is not wrong btw) and provide the opportunity to save the solvent for future use. But yet again this is an individual preference and by all means not the only approach to this conversion.

Your understanding about reaction and precipitation is right, I might have misused the (/) but precipitation occurs upon the reaction of the 2 molecules forming bonds. That was my point and sorry if it sounded a bit misleading.

Usually I used to add FASI as slowly as possible to aid in pretty xtal formations, and of course there is nothing wrong with rigorously shaking the soln, it just puts out a slightly different end result.

Anyway, nice results and I did not want to point out in no way that your procedure is wrong. Accept my apologies if that's the way I sounded.

Also one good way to test your fumarate is to taste them. DMT fumarate should be bitter as opposed to fumaric acid which has a sour flavour to it.

 

[Levanah]

In theory and also in regards to my advise to precip over evap, the idea was that any soluble impurities (or excess f.acid) present in the used starting material would remain suspended in soln, and decanting that off of the fully precipitated crystals would only result in a higher purity for the alks.

Thank's a lot, I undertand your point. I'll go the precip route next time I convert some of my brown full sprectum oil into fumarates. Can't wait to see the results. Peace!

 

[downwardsfromzero]

Check the solubility of fumaric acid in IPA; there's nothing wrong with using 618 mg per 100 mL (I love how that's the golden ratio or thereabouts, btw!) but that figure is for acetone. You'll be able to dissolve a bit more in IPA and thus use less solvent - which has its pros and cons as well.

Also bear in mind that 99.99% IPA will be hygroscopic and absorb water from the air fairly quickly, to the eventual tune of 9%. After a while you'll have 91% IPA but at least the remainder will be virtually all water. Damp IPA is a somewhat better solvent for DMT fumarate. That is to say (and maybe you know this already) you'll be wanting to dry your solvent after a while.

If you perform this procedure a second time, save some of those beautiful, sparkly crystals of yours to use as seed crystals for the next batch. Things may well precipitate more quickly and the crystals should be bigger too. Larger crystals may have some advantages.