More issues trying to make Fumarate.

[Violet Quark]

Hi Folks
I've been trying to follow this method again to make DMT Fumarate.

The FASA Method - DMT-Nexus Wiki

wiki.dmt-nexus.me

It's not gone as planned and could use some advice as I'm clearly doing something wrong.
I dissolved about 1.5g of DMT int 99% Acetone straight from an unopened bottle.
I then made some saturated FASA solution in the same Acetone. I have to admit I used way too much Fumaric acid here but I thought that more was better than less since it will only dissolve until it's saturated any way.
I dropped the FASA into the DMT solution until there was no more precipitate.
I dried this and it produced about 600mg of yellowish brown powder as seen here.

I'm sure this is DMT Fumarate.

Obviously there was a lot of spice missing so I added to more Fumaric acid directly in the jar with the dissolved DMT thinking it would precipitate into Fumarate but nothing happened.

I then evaporated the entire jar of dissolved DMT/Fumaric Acid and got 1.9g of yellower powder as seen here.

This is now clearly a mixture of Spice, DMT Fumarate and Fumaric acid because it weighs more than what I started with

My questions are:-

Is the first powder really Fumarate?
If it is, why didn't more Fumarate precipitate out in the first place?
What is the best way to go forward with the mixture I have? I mean how can I separate it it out?
Can I dissolve it Naphtha to get the DMT out and leave the rest behind or something.?

Any help much appreciated.

 

[Transform]

Hi Folks
I've been trying to follow this method again to make DMT Fumarate.

The FASA Method - DMT-Nexus Wiki

wiki.dmt-nexus.me

It's not gone as planned and could use some advice as I'm clearly doing something wrong.
I dissolved about 1.5g of DMT int 99% Acetone straight from an unopened bottle.
I then made some saturated FASA solution in the same Acetone. I have to admit I used way too much Fumaric acid here but I thought that more was better than less since it will only dissolve until it's saturated any way.
I dropped the FASA into the DMT solution until there was no more precipitate.
I dried this and it produced about 600mg of yellowish brown powder as seen here.
View attachment 104794
I'm sure this is DMT Fumarate.

Obviously there was a lot of spice missing so I added to more Fumaric acid directly in the jar with the dissolved DMT thinking it would precipitate into Fumarate but nothing happened.

I then evaporated the entire jar of dissolved DMT/Fumaric Acid and got 1.9g of yellower powder as seen here.

View attachment 104795This is now clearly a mixture of Spice, DMT Fumarate and Fumaric acid because it weighs more than what I started with

My questions are:-

Is the first powder really Fumarate?
If it is, why didn't more Fumarate precipitate out in the first place?
What is the best way to go forward with the mixture I have? I mean how can I separate it it out?
Can I dissolve it Naphtha to get the DMT out and leave the rest behind or something.?

Any help much appreciated.

Firstly, it would be helpful to have some figures to complement the qualitative account that you've given. That way, you'll be able to work out how much yield to expect from the second, evaporated batch.

Next, do you think there was any guarantee that your fresh bottle of acetone hadn't absorbed moisture during storage? It may have been more prudent to have attempted chemically drying it before use, especially since acetone can generate a little water autogenously through self-condensation.

Your second batch, which surely contains some excess of fumaric acid, however small, can be recrystallised using boiling anhydrous IPA. This should remove the excess of FA if you use sufficient solvent.

 

[Violet Quark]

Hi Transform
Thanks for the reply.
I'm sure the acetone was pure, it was 99% and sealed. I have since added a load of atomic sieve to it so it will be 100% next time, hopefully anyway.
I wasn't expecting so many problems, which is why I didn't really weigh everything beforehand.
I have now ordered 100mm 0f 99.9% IPA.
I am planning to boil this in a water bath, add the powder, decant the liquid and then evaporate the IPA.
Is that the correct procedure?
Also, how will I know if I have Spice or Fumarate?
Can I dissolve the residue in Hexane? As I understand it this will dissolve the freebase but leave the fumarate behind. Does this sound right?
Thanks for again the help.

 

[Transform]

I am planning to boil this in a water bath, add the powder, decant the liquid and then evaporate the IPA.
Is that the correct procedure?

Not quite. Everything should dissolve on boiling with sufficient IPA, but the DMT fumarate will crystallise back out on cooling. Do not evaporate it down! The fumaric acid will stay in solution - unless you've added a really large excess of it. (In this latter case, you'd have to perform a second recrystallisation with fresh IPA, or after recovering your IPA by distillation.)

The recovery of your DMT fumarate can be maximized by chilling the solution. Then you can filter off the crystals and give them a rinse with fresh, chilled IPA.

An alternative, requiring less solvent, is to rinse the crystals as you have them at present with clean acetone or IPA, taking care to minimise exposure to atmospheric moisture. This won't get rid of excess FA trapped in the crystal matrix, however.

 

[Violet Quark]

OK Thanks I'll give this method a try when the IPA arrives.