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Just throwing Fumaric Acid right into the DMT/Acetone - possible?

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Brennendes Wasser

Brennendes Wasser

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Senior member Chemical engineer
Hello!

So yes the Fumaric Acid was said to should fully dissolve in Acetone prior to throwing it on the DMT/Acetone.

This sounds logically as an already solvated Molecule can immediately react / precipitate with that other one and the precipitation will be very nicely.

But I have witnessed that the solubility of Fumaric Acid is still quite poor in Acetone.



Now I want to convert a big pile into the Fumaric Salt.

This would need way too much Acetone to fully dissolve it ... now I did not do any Maths but I just assume it.


My Idea:


Fully dissolve Spice in a bigger amount Acetone (easy ...)

then

throw the needed amount of Fumaric Acid right into it and then stirr (+ maybe heat it a little) for like 1 hour maybe ...



So in theory: A little Fumaric Acid gets dissolved and then IMMEDIATELY crashes out ... then the equilibrium will make more Fumaric Acid dissolve and so on and this would surely be finished after like 1 hour to wait.

So does anyone have ANYTHING to say against this?

Any reason why fumaric acid must DEFINETLY be fully dissolved in the first place and it won't work otherwise ?


THXXX
 
I think the spice solution also needs to be saturated, or at least as concentrated as possible.

Otherwise the reactants will stay dissolved after part of it crashes out - I think FASA works because we move on the edge of solubility curve.

It will be probably hard to dissolve any fumaric acid in already highly concentrated spice solution - if it will dissolve at all. You really need that little excess of acetone but then it will be even harder not to overshoot it.

You would also end up with excess fumaric acid in the product this way. This can fixed later by washing with ice cold acetone though, but lots of fumaric = lots of extra struggle.

I also had bad results with room temp. acetone. I had to chill both FASA and spice solution as otherwise some stuff stayed in acetone. This is harder to achieve when you want long stirring.

But there is only one way to know :) Will you try it?
 
It seems not much is dissolving but it is.

1g fumaric acid dissolves in a little bit less than 100ml of acetone (source)

Freebase DMT molecular weight is 188.269. Fumaric acid weight is 116.07. DMT fumarate has a molecular weight of 492.608 (DMT + fumaric acid + DMT)

That means fumaric acid is around 38% of the weight of DMT fumarate. So 100ml FASA should be enough to salt out more than 2.6g DMT.

Do you still think you will need too much acetone to dissolve your pile?

As for putting fumaric acid directly, it's probably not a good idea as Mindlusion already explained elsewhere. Fumaric acid is a diprotic acid, but due to equilibrium, if you add too much fumaric acid at once it may theoretically form a monoprotonated salt. Generally these salts do not store well, being hygroscopic, do not crystallize easily and can degrade.

So you want to do FASA the right way.

Or... You can do partly the right way and partly the wrong way, and then see what happens and let us know the results :D
 
Brennendes Wasser said:
Hello!


Any reason why fumaric acid must DEFINETLY be fully dissolved in the first place and it won't work otherwise ?


THXXX
Click to expand...

Yes there is a reason.
At the end of your proposed process, you will have a solid. And then you have no way of knowing if your solid is dmt fumarate or dmt fumarate plus a quantity of fumaric acid. Then what?

I think you will feel far more satisfied using the proven method, knowing that your product is free of fumaric acid.

Hope that helps.
 
leratiomyces said:
Yes there is a reason.
At the end of your proposed process, you will have a solid. And then you have no way of knowing if your solid is dmt fumarate or dmt fumarate plus a quantity of fumaric acid. Then what?

I think you will feel far more satisfied using the proven method, knowing that your product is free of fumaric acid.

Hope that helps.
Click to expand...


Yes!

Also, the slower you add fumaric acid (solution), the bigger nicer and seemingly purer DMT fumarate crystals form.
 
You can heat up both acetone parts, so there will be more fumaric acid dissolved.
Click to expand...

Yes while I did some minor stuff with Fumaric Acid, what made me believe is dissolves pretty bad, I heated it to boiling of course ;D

Still I haven't done it with the desired amount I talk about.


At the end of your proposed process, you will have a solid. And then you have no way of knowing if your solid is dmt fumarate or dmt fumarate plus a quantity of fumaric acid. Then what?
Click to expand...

Well so in case that uncertainty is caused because of excessive Fumaric Acid -> I would only use the correct amount.


Then one may argue I don't know whether the reaction is complete, but as I said I would just let it stirr for 1 hour or maybe even 2.

And just by thoughts: If the Fumaric acids dissolves slowly (I guess you don't need 20 minutes to dissolve all your stuff), then it will still dissolve permanently and crash out. So this will be a constant process. I would really not consider that it is that slow that I cannot just stirr it for 2 hours and then it wouldn't be complete.



But yes: I WILL try both methods ;D

I may test if the other method just yields Fumaric Salt + still free Fumaric Acid if I can dissolve some back with Naphtha (which would dissolve the free DMT) and then the weight would be lower.
 
I dont need crystals, I prefer powder. And my entry freebase is already of required purity. So I go ahead and put the saturated heated fum acid acetone into saturated heated dmt fb acetone within a minute. I use about 5-10% more fumaric acid than required by calculation. The result is powder of expected weight. After tone evap nothing interesting remains
 
Just over saturate a bottle of dehydrated aceton with FA, leave it for a couple of days and filter the remaining FA out. Clear FASA.

Any other way is more complicated. You mention FA dissolves difficult. Indeed, this is the reason your method will risk having undissolved FA in your DMT Fum. More work, more FA residue risk. No point.
 
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