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FASA - lost over 50% yield AGAIN Options
 
blue.magic
#21 Posted : 12/28/2017 4:52:50 PM

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Loveall wrote:
blue.magic wrote:
...I decanted the solution and washed several times with fresh acetone.


Sorry if this has been asked before, but was this fresh acetone anhydrous?


It was as dry as a Sonoran desert. Please note the losses happened repeatedly, even with new reagent-grade acetone.


Lessons learned:

- weigh material BEFORE washing
- use ice cold acetone/MEK for washing
- weigh material AFTER washing
- if there is significant difference, recover DMT from the washes and repeat the procedure
 

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Infundibulum
#22 Posted : 1/7/2018 2:36:45 PM

Kalt und Heiß, Schwarz und Rot, Kürper und Geist, Liebe und Chaos

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blue.magic wrote:
I used 300 mg of very pure (recrystallized) DMT. I followed the FASA method from Wiki to the letter. The only exception was that I washed the DMT fumarate with fresh acetone several times (always let the fumarate to settle and decanted the supernatant liquid) to remove any excess fumaric acid and make sure the result will be DMT fumarate only.

And still I was left with only 176 mg of DMT fumarate, that is about half of the original weight of DMT. Since fumarate is heavier than freebase, I expect to still get around 300 mg of fumarate even when losses are present.

I am really tired and a bit angry. Why am I losing so much product every time?? I am not sloppy and tried the method several times, gone through tutorials on analytical methods and did everything to prevent losing HALF of the product. For example:

- prepared fresh anhydrous magnesium sulfate
- prepared fresh anhydrous acetone
- oven-dried absolutely everything (including bottle for the anh. acetone)
- flame dried every piece of glassware before use

Yet every time I make DMT fumarate using the FASA method I somehow lose over 50% of DMT.

How do you make DMT fumarate and prevent these huge losses and what could went wrong?

I am getting hopeless, checked and re-checked every step and still every time I work on my DMT, be it purification or FASA, over half of it simply disappears into nothingness...

Hi blue.magic,

I understand your frustration - from my and many other people's experience the weight math of freebase to fumarate and vice versa normally works out as expected.

Could in our case the loss of be actually a non-loss? In other words, you say that you started with "300 mg of very pure recrystallized DMT". Was that DMT crystals or was it dmt powder?

My understanding is that those oh so beautiful dmt crystals trap solvent (naphtha) and are heavier that they should. Crystal formation and shape is solvent-dependent (among other things of course) and solvent molecules are known to often form part of the molecular crystal lattice to e.g. influence crystal shape.

So if you started with dmt crystals I'd be inclined to believe that you had less than 300 mg to begin with and that now you have a purer form (dmt fumarate), and taht would explain the greatest part of the weight discrepancies observed.

If however you did start with a thoroughy solvent-free dmt preparation, that was powdered and then further left so as all traces of (re)crystallisation solvent evaporate, then I truly do not have an explanation with the current data you have provided. But we can get to the bottom of this if you are willing to perform a few more diagnostic tests/experiments.





Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
blue.magic
#23 Posted : 1/7/2018 10:58:01 PM

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Infundibulum wrote:
Could in our case the loss of be actually a non-loss? In other words, you say that you started with "300 mg of very pure recrystallized DMT". Was that DMT crystals or was it dmt powder?

My understanding is that those oh so beautiful dmt crystals trap solvent (naphtha) and are heavier that they should. Crystal formation and shape is solvent-dependent (among other things of course) and solvent molecules are known to often form part of the molecular crystal lattice to e.g. influence crystal shape.


Yes, this is very possible. I will try some kind of vacuum drying when I get a strong enough pump for a water aspirator. I have a vacuum dessicator, but it's pain to work with (the two glass parts always stick together no matter how much grease I use).

As for the solvent, I used 99.8% n-heptane (for synthesis), but the crystals formed look just like from naphtha (Zippo). I am thinking about using different tek when targeting fumarate (backsalting from NPS, saving the DMT step).

The crystals are tiny and fluffy, I never thought about powderizing them. Will try it next time. Thanks.

Sure, apart from the above precautions, I will weight the intermediate product and track partial yields to spot any losses.
 
blue.magic
#24 Posted : 1/18/2018 6:37:23 PM

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Okay so this time I've used ice cold (-18 C / -64 F) acetone and FASA for making DMT fumarate.

I started with approx. 520 mg of DMT recrystallized from heptane.

It took about 5 ml of FASA until the fumarates crashed from the solution. Filtered, dried and scraped approx.430 mg of fumarates.

I ground the fumarate powder so it can be washed more easily. I was left with 425 mg of fine powder.

After washing with fresh ice cold acetone, filtering (vacuum with glass micro-fiber filter) and drying (20 minutes at 80 C / 176 F), I was left with 361 mg of DMT fumarate.

I don't know if such yield is normal, but it's definitely way better than last time. Using ice cold acetone seems to matter a lot. Of course, there are inherent losses in the process, the source material is not pure. Next time I won't filter it, only wash once of twice with acetone and left to evaporate the solvent, which should reduce the number of transfers.

In the end, I am quite happy with the result and will try this with a sitter.

I am thinking about taking 230 mg of harmine hydrochloride followed by 65 mg DMT fumarate (spaced by 20 minutes).

Unfortunately, the pharmahuasca dosages are very broad and sometimes they refer to just "DMT", not specifying the salt type, giving extra margin of error. I hope I won't underdose or overdose myself because of that...
 
Jees
#25 Posted : 1/19/2018 11:27:19 AM

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blue.magic wrote:
...Unfortunately, the pharmahuasca dosages are very broad and sometimes they refer to just "DMT", not specifying the salt type, giving extra margin of error. I hope I won't underdose or overdose myself because of that...
You're in the right ballpark. The success of an experience is only partly dose dependent, so deems salt or deems FB is not going to make a huge difference imho. On some occasions it even seems dose independent LOL. What does make the difference is the assimilation speed of the digestion track. We only have a few handles on that one, like empty stomach. When it gets assimilated fast it hits like a truck, and sometimes it is so spread out that the peak level is flattened, it's always a bit of surprise for me. But in the morning after a night sleep I've found largest intensity and prolonging at same time, but we all differ, just sharing.
 
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