First FASA Attempt - Low Fumerate Yield (.45%)

[Complexity]

Hello, as announced in a bad written topic some weeks ago, I've performed a FASA. My yield though hasn't been satisfying, and I would like to see where there's room for improvement.


I prepared a FASA solution and a solution of acetone and citric acid (should have been 5g/100 ml, but this could be debatable... even if honestly it's more likely to have been more than 5g). The FASA was left several days to absorb as much fumaric acid as possible, even stirred for a whole afternoon, and in the end there was still fumaric acid at the bottom.

I powdered 10g of MHRB for about 1-2 minutes in a coffee grinder.

I stirred the plant for 2h in 40ml of the acetone+citric acid solution. x3 total. Filtered and combined. I notice a significant decrease in the volume.

Added something like 120 ml of FASA (which seems to me an overkill). Covered with plastic wrap, put a bigger beaker with the mouth oriented towards the ground to contain the one containing the solution. (Hope the explanation is clear). I did this hoping to protect the solution from moisture (I live in a pretty humid area).

Waited 3 days. Collected 45 mg of DMT fumerate.

Something done wrong? Bad plant material?

I want to try to add more FASA, just in case.


Thanks for the attention!

 

[downwardsfromzero]

Your method was completely awry, it's amazing that you recovered anything! What information was your method based on?

I'm not convinced you'll pull much from bark with citric/acetone. DMT citrate is only poorly soluble in acetone, IIRC. With the caveat that most citric acid is sold as the monohydrate. Anhydrous citric acid is (or was) available as a descaling agent. So if any of us were wanting to use properly anhydrous solutions of citric acid this sort of thing should be useful to know.

The humidity most assuredly hasn't helped, you'll want to build a makeshift desiccator. Think plastic tub with anhydrous calcium chloride or silica gel. Needs to be big enough for your solvent container, naturally.

I'll wager that most of the goods are still in the bark and anything else is in your damp acetone. Otherwise your bark is bunk.

 

[TGO]

The above method may have been taken from here:

Spoiler

A Safer DMT Extraction - No Lye, No Naphtha

For one thing, it inspired a DMT extraction that doesn't require any lye or hydrocarbon solvents (like naphtha, toluene, etc.). This tek uses only citric acid, fumaric acid, acetone, sodium carbonate, and water. This makes it much safer for the layman than playing with strong lye solutions and being exposed to the vapors of hydrocarbon solvents.

The purely imaginary method described below does work, but it works really really slow. SWIM's FOAF was able to extract ~100mg freebase alkaloids from 10g of MHRB. This method does not discriminate between the alkaloids that are extracted (j.spice, d., d-Noxide etc etc), this is however a subject of discussion.

The tek:

1) dissolve 5g of citric acid per 100ml acetone

2) take the shredded/powdered bark and cover it with enough citric acid acetone. Incubate in a warm place, gently agitating every so often. After 2-3 hours, filter off the citric-acid saturated acetone extract and set aside (this solution should have acquired the dark reddish colour of MHRB). Repeat 2 more times.

3) saturate acetone with fumaric acid. Acetone can hold ~20mg/ml fumaric acid if let for a day or so to completely dissolve.

4) Add the fumaric acid-saturated acetone in the citric acid-saturated acetone MHRB extract. One cannot put too much.

5) Set it aside and wait for 2-3 days. One should see a yellowish precipitate on the bottom.

NOTE: In step 2 one is making an acetone extraction and at the same time converting the alkaloids their citrate salt. After addition of the fumaric acid-saturated acetone in step 4, there is an interconversion of alkaloid-citrate to alkaloid-fumarate salt, like:

dmt-citrate + fumaric acid <-> dmt-fumarate + citric acid

citric acid has a pKa of 3.13, while fumaric acid's pka is 3.43. Fumaric acid is a weaker acid and thus in the above reaction one should have most of the dmt as a citrate salt and just a tiny amount as a fumarate salt. dmt-fumarate however is totally insoluble in acetone (while dmt-citrate is perfectly soluble), and it precipitates as soon as it forms. The insolubility of dmt-fumarate acts therefore as a "sink" and given time all of the dmt-citrate will eventually convert to dmt-fumarate and precipitate out.

6) wash the precipitated fumarate salts with acetone, then take them out and let them dry.

7) dissolve the alkaloid-fumarate salts in 5ml of tap water, then and then add saturated sodium carbonate to make the solution basic. The alkaloids will be freebased and the solution will become milky. In 3 days they will precipitate out forming nice needle-like crystal in the basic solution. At this stage, one can filter the solution (nasty procedure since the crystals tend to be sticky and waxy) and retrieve any left alkaloids by dissolving them in acetone.

8 ) Let the crystals dry, wash them with acetone (it removes any traces of sodium corbonate which is totally insoluble in acetone), evaporate the acetone and enjoy the product.

For the FOAF of SWIM 30mg were for a good STRONG experience.

The above tek was quoted from here: The FASA Method: A Summary - DMT Fumarate and Beyond - FASA/FASI/FASW - Welcome to the DMT-Nexus

 

[Complexity]

Yes it was taken from there.

Funny thing is that I discarded the idea to use citric acid time ago, then after a series of weird reasoning I decided to use it again.
At least my citric acid was anhydrous

But so, would an extraction into plain acetone work? I mean, in the plant we have dmt-tannate right? Isn't it insoluble in acetone?

 

[downwardsfromzero]

I mean, in the plant we have dmt-tannate right? Isn't it insoluble in acetone?

I'm not sure we even know. Chances are about evens that it's soluble as that it's insoluble. A vinegar (or better, acetic acid) soak followed by drying then pulling with acetone should eliminate that ambiguity.

FASA might not precipitate terribly well if your acetone is too damp so eliminate that variable first, if you believe the tek to be sound.

On a sideline, I've found an OTC source for both 60% acetic acid and acetone locally so I may try this out just to see. (As you may infer, I have the anhydrous citric already ) Trying the procedure with plain acetone, and maybe also with a vinegar/sodcarb pre-process, would be variations worth investigating.

One final question: you did dry your acetone thoroughly, didn't you?

 

[Complexity]

I mean, in the plant we have dmt-tannate right? Isn't it insoluble in acetone?

I'm not sure we even know. Chances are about evens that it's soluble as that it's insoluble. A vinegar (or better, acetic acid) soak followed by drying then pulling with acetone should eliminate that ambiguity.

FASA might not precipitate terribly well if your acetone is too damp so eliminate that variable first, if you believe the tek to be sound.

On a sideline, I've found an OTC source for both 60% acetic acid and acetone locally so I may try this out just to see. (As you may infer, I have the anhydrous citric already ) Trying the procedure with plain acetone, and maybe also with a vinegar/sodcarb pre-process, would be variations worth investigating.

One final question: you did dry your acetone thoroughly, didn't you?

Well, first I'll give a try with just acetone (actually I tried already... but at a certain point I discarded everything because I felt sure it couldn't work), then even the vinegar soak sound promising.

My acetone was sold to me saying it has at most 0.5% water.
I also already have acetic acid, probably above 60% (can't recall actually)

I don't live in the USA, here it's quite easy to get a lot of stuff!



Thanks for the answers

 

[downwardsfromzero]

I don't live (and have never lived) in the USA either, but I recently moved to a different country and finding new supplies has been an adventure. I'm still adjusting to the difficulty of finding pure caustic soda OTC without questions! It's fun to be inventive while learning everything in another language.