Hello there,
is it possible to solve unclean dmt freebase in naphta, adding then slowly tiny amounts of HCl to precipitate pure dmthydrochloride?

You mean 35% HCl? I think the salt will go into the tiny water layer and stay dissolved in there.

If you dissolve the DMT in dry alcohol and then add small amounts of 35% HCl you may get some precipitate as the water will be busy with the alcohol. Seems to work for mexamine precipitation for example.

ah okay, is it possible to do all this in acetone?

I wouldn't recommend it as HCl can react with acetone, but I'm not really sure what would happen.

This is basically called "mini A/B" which purifies the product very well.

If you have or can make dry (anhydrous) acetone, you can go for DMT fumarate (The FASA Method). Acetone is pretty good solvent so it can hold lots of impurities and you have an opportunity to wash your fumarate several times, purifying it even more.

The HCl backsalting is also viable option. Some people go for toluene as a solvent, since it dissolves more impurities than naphtha.

I usually recrystallize from heptane just once, the product is pure enough for most uses.

Thanks (also for reminding at fumarate, nearly forgot about it)
Yes backsalting is what i mean, should have named the post so

Does backsalting in naphta with HCl really work? Will the HCl dissolve in the naphta?

I guess acetone works much better?


what exactly do you mean by recrystalization from heptane?

35% HCl in naphta should simply make a separate acidic water layer where the DMT salt is in solution.

If you are really interested in how HCl could work with naphta to precipitate DMT HCl salt, I've heard (but not verified) that using a dry HCl gas bubbler may do the trick. However that is something for a professional lab, not for a home alchemist should actually try to do in my personal oppinion.

Safety first

ah
when i make a citric acid acetone solution will it be acidic enough to convert the dmt freebase back to its salt?

Citric acid is acidic. That's why it's called citric, uh, acid.

It has protons which relatively easily can be donated to the basic nitrogen atom of the amine functionality of the DMT molecule. It will do the job, and form protonated DMT cations. These will combine electrostatically with the resulting citrate anions (in the absence of solvating water molecules), leading to the precipitation of crystals of DMT citrate.

There are a couple of things to bear in mind when using citric acid:

Citric acid is tribasic, meaning it can combine with one, two, or even three molecules of DMT freebase. This means there are potentially at least three possible forms of DMT citrate.

Citric acid is commonly encountered as the monohydrate for food usage. To ensure success when attempting to precipitate from acetone, it's best to take meticulous steps towards anhydrous conditions. Rather than trying to dry out your citric acid, you may prefer to find anhydrous citric acid, which is sold as a food grade descaling agent.

Thirdly, because of these factors, you will want to do some careful calculations to ensure that you are using sensible proportions of citric acid to DMT.

I was thinking of the HCl bubbler and had a separate thought.

What would happen if fumaric acid is added to naphta that has DMT? Would a slow and steady conversion to DMT funarate occur? Here is a thing that may be worth trying:

- Start with naphta DMT frebase solution
- Add funaric acid in slight excess
- Let it sit for a day with regular shaking or for a few hours on a stir plate. Adding a small ammount of dry acetone/IPA may help speed up (or start) the reaction.
- Decant naphta

Two options now:

Cleanup 1)
- Dissolve solids in water
- Water may have a top layer of residual naptha, remove that (e.g. use a syringe to suck up the top layer, alow the syringe liquid to separate and put the bottom water layer back in).
- Filter water and dry.
- Any DMT funarate?

Cleanup 2)
- Rinse in dry acetone or IPA until the wash evaporates clean.

This is just FASW or FASI/W with a couple steps swapped. Separation of the two layers is less bulky this way vs FASW (if it works) or potentially less Acetone/ILA is used.

Anyone try something like this? Thank you.

@downwardsfromzero thank you, i will get pure citric acid, sold as descaling agent, and use dried acetone
yes, i tried before some calculations to prepare citric acid solution and it was quite a hassle. When i prepare a acetone citric acid solution, can i use the same proportions as with water? For example 30 gram of citric acid in 1 gallon of liquid (water in the recepy, in my case acetone) like in Shaggy's Jungle Tek?

DMT freebase is extremely soluble in ethanol. I don't know about the solubility of DMT HCl in ethanol, but it's a good question. I will test this with anhydrous HCl gas and get back to you. I will also test it with d-tartaric acid to see if the DMT tartrate will precipitate out from the ethanol. Stay tuned for the results.