Author Topic: Entropymancer and friends present : The FASA Method!  (Read 581 times)

agmotes165

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Entropymancer and friends present : The FASA Method!
« on: February 15, 2009, 05:03:32 AM »
A brilliant person that has helped us all with everything from Mescaline to LSD to DMT...all I am doing is passing on his info.
ALL CREDIT FOR THIS GOES TO ENTROPYMANCER FROM THE SHROOMERY




The FASA Method: DMT Fumarate and Beyond

("FASA" stands for Fumaric Acid Saturated Acetone. I'll use that acronym throughout this post to refer to anhydrous acetone that has been saturated with fumaric acid. 100 mL of acetone can dissolve about 618 mg of fumaric acid)

I had no involvement in discovering the methods described below; many thanks go out to Infundibulum, 69Ron, amor_fati, and all others who have helped in pioneering these developements. All credit goes to them.

I just thought that the FASA method deserved its own thread (might be worth stickying?). It really seems like it's the future of DMT extractions. It's led to the developement of an extraction tek that doesn't use lye, naphtha, or xylene/toluene/etc. That's a huge plus in terms of making extractions safer (people don't have to worry about handling caustic lye solutions and naphtha fumes). And the xylene/FASA method seems like an improvement over naphtha extractions for people who still want to use lye-based teks (xylene/toluene are better solvents than naphtha, but you can't freeze-precipitate and evaporating them was a pain in the ass).

All the info here was compiled from two threads: Pure DMT Fumarate from freebase DMT and Discussing Alternative Spice Extraction Techniques. I've just trimmed out all the really juicy bits from the threads and put it all in one place for easy reading.

Personally, I had stopped checking the 'Pure DMT Fumarate from freebase DMT' thread after the initial discussion of precipitating DMT fumarate from acetone. I had no idea how many new developements I was missing! I'd seen the term "FASA" getting thrown around, but it took some searching for me to figure out what it was referring to.






Here's a quick summary of what this covers:
* An easy way to make DMT fumarate from freebase DMT
* A DMT extraction method that doesn't require lye or typical hydrocarbon solvents
* Two ways to convert DMT fumarate to freebase DMT, neither one using lye or hydrocarbon solvents
* A way to obtain DMT (and other "jungle spice" alkaloids) from xylene or toluene without evapoting
* A potential improvement to mescaline extraction teks (still needs to be tested)







Freebase DMT to DMT Fumarate

Initially, some folks discovered that if you dissolve DMT freebase in acetone and add FASA, DMT fumarate will precipitate out of the solution. While DMT freebase is soluble in acetone, DMT fumarate is not.

69Ron wrote:
Here’s the quick tech:

1) Completely dissolve 1000 mg of freebase DMT in 50 ml of acetone.
2) Completely dissolve 309 mg of fumaric acid in another batch of 50 ml of acetone.
3) Mix for 1 minute and evaporate at room temperature to give DMT fumarate.


Now that's kinda neat in itself, it provides an easy route to the one salt of DMT that's known to exist stably as a solid. Regarding DMT fumarate, 69Ron commented:

69Ron wrote:
DMT fumarate forms completely colorless, long clear pointed crystals in MEK that look like the kryptonite crystals seen in the superman movies. They will be lightly yellow or amber colored if impure.

DMT fumarate is best for snorting, taking sublingually, injecting, taking intra-rectally, or taking orally with an MAOI. If a person wants to smoke DMT, they need freebase DMT. SWIM thinks smoking it is a waste. The trip is too short. SWIM prefers the other routes of administration because the trip is much longer lasting.


Infundibulum got curious and did some solubility testing of DMT fumarate in different solvents:

Infundibulum wrote:
5ml of methanol, ethanol, isopropanol or ecetone were saturated with SWIM's dmt fumarate, then the solvent siphoned off and evaporated. The residue was weighted. The results are:

Acetone : practically 0mg/ml (there was a very thin layer of residue left, impossible to scrape

IPA : ~1mg/ml. The residue was still too little to be weighted properly

Ethanol : ~5mg/ml

methanol: ~10mg/ml


This discovery opened the way for several other developements.







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.

Infundibulum wrote:
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.









DMT Fumarate To Freebase DMT - Two Methods Without Using Lye or Naphtha

You'll notice that step 7 is quite a developement in itself: For the first time, someone has presented a viable method for crystalizing freebase DMT out of water. Infundibulum also posted a pictorial of step 7, showing the formation of the DMT freebase; this has been attached as a pdf.

Of course, that method can be a bit messy, so for those disinclined to attempt it, there's an alternate method of converting the fumarate to freebase without using any nonpolar solvents (of course dissolving the fumarate salt in water, basifying to pH 10+, and extracting with naphtha works as well):

69Ron wrote:
1 - Mix DMT fumarate with 1 part calcium hydroxide (calcium carbonate should work as well).
2 - Add enough water to make it wet and mix. (Freebase the DMT again)
3 - Spread it out and let it dry completely.
4- Dissolve it in acetone and filter out the solids. (At this point only alkaloids like DMT should dissolve)
5- Evaporate the acetone to get nearly pure freebase DMT.









FASA Method Precipition From Xylene - No More Need to Evaporate!

But new methods of extracting spice without using lye or hydrocarbon solvents wasn't the only developement this inspired. Some intrepid experimenters also discovered that FASA can also be used to precipitate DMT out of some other solvents besides acetone! This was initially discovered with xylene (again, posted by Infundibulum):

Infundibulum wrote:
a) first xylene pull (coloured piss yellow) goes in an appropriate container.

b) FASA was added dropwise, xylene became cloudy due to the salted alkaloids. One cannot put too much FASA.

c) solutions was left overnite at room temperature allowing for the alkaloid-fumarate to sediment. Now one got them out of the xylene without the need to evaporate it!

d) Xylene was siphoned off and washed with plenty of water. This was done because this xylene had traces of acetone and fumaric acid that one does not really want. Water washed away fumaric acid and acetone, leaving back clean xylene (plus the yellowy plant oils that dissolved into it). This xylene was used for the second pull etc etc. By this approach one knows when to stop pulling since at some point there will be no alkaloids in the xylene to be salted out. it took SWIM 7 100ml xylene pulls to exhaust 240g MHRB.

e) fumarate alkaloids were washed 3 times with some acetone to remove any residual xylene and oily impurities.

f) Then they were dried in the oven at 70 Celsius until pretty hard.


This is a great developement! It circumvents the tedious process of evaporating xylene. Since the "jungle spice" alkaloids seems to precipitate as the fumarate as well, this will save jungle spice extractors a lot of time. And from an economic standpoint, this allows the same batch of xylene to be re-used repeatedly for subsequent pulls. If I ever get around to extracting another batch of spice, I'll probably use xylene for all my pulls.

This method of precipitating the fumarate salt from nonpolar solvents has been confirmed to work with both xylene and toluene. It does not work with "Bartoline Premium Low Odour White Spirit" (when the FASA is added, the fumaric acid precipitates immediately, not DMT fumarate); it therefor seems likely that the FASA precipitation would not work with typical naphtha extractions (but we can freeze-precipitate from naphtha, so there's really no need for it). If anyone cares to try, it would be useful to know whether this method of DMT fumarate precipitation might work with DCM, or d-limonene.








Theoretical - An Improvement on Mescaline Extractions?

Lastly, one more implication needs to be investigated. If mescaline fumarate is insoluble in xylene and toluene, then it seems quite likely that the FASA precipitation method would greatly simplify mescaline extractions. No more careful titrations; no more guessing how much mescaline is in there and adding an appropriate amount of acid to obtain the salt. Just add some FASA to the xylene or toluene extraction, and out crashes mescaline fumarate! If anyone is doing a mescaline extraction at the moment, I highly encourage testing this.







Some Basic Info on Fumaric Acid and Anhydrous Acetone

Fumaric acid is used as a pH adjuster in the winemaking business, so check your local winemaking/homebrew shop to obtain it. If you're in the US, it can be ordered online. (No sources are allowed on this board, but check for links at the bottom of this thread)

Most people trying these methods will be buying acetone from a hardware store. Hardware store acetone is generally not anhydrous, it contains some amount of water and/or alcohols. Amor_fati provided a link from bluelight that describes how to dry your hardware acetone using epsom salts.

Quote:
You can easily turn hardware store acetone into anhydrous acetone with the simple process I've outlined below. To do this, you'll need to go to Home Depot or Lowes and get the following items: a 1 liter can of acetone and a bag of epsom salts.

Heat some epsom salts on an aluminum foil covered baking sheet in the oven for 2 hours at 400 degrees F. After 2 hours of heating, the epsom salts have now been turned into anhydrous magnesium sulphate. Crazy huh?

Take 10-20 grams of your greyish ash looking anhydrous magnesium sulphate and pour it directly into your can of hardware store acetone. Shake the can vigorously for a few minutes to circulate the magnesium sulphate and then let it settle for 24 hours. The magnesium sulphate will absorb all of the water and/or alcohol from the hardware store acetone and sink it to the bottom of the can where it shall remain forever.

Therefore from now on, never pour from the can, instead use a glass eye dropper or glass pipette (glass straw) to reach down inside of the can to extract however much anhydrous acetone you'll be requiring. Always stay away from the bottom of the can. Once the can get's about half way down, discard and repeat the process with a fresh can of acetone. Always use glass hardware when using acetone. Acetone will melt plastic.

Peace to all them kids...
agmotes165

Vesp

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Re: Entropymancer and friends present : The FASA Method!
« Reply #1 on: March 24, 2009, 11:48:04 PM »
Is there an easy to get alternative to fumarate? would something like glutamic acid work?
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poorfish

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Re: Entropymancer and friends present : The FASA Method!
« Reply #2 on: January 12, 2011, 10:35:26 PM »
Old thread bump I guess, but were you having trouble sourcing fumaric acid?  

It seemed quite easily available the last time this wasp checked...I believe it is used somehow in the process of making wine (not sure how, but its generally in-stock in specialty wine stores or from a hobbyist/home brewer's outlet)

'Course there's also zee internets....if you're familiar with *No Sources Allowed* they usually have it, although they seem to make a policy of stocking such items in small amounts for higher prices than totally necessary.  Just checked 'n they has it for $3/ounce before shipping....not that great if you're looking to saturate anything with it.  

But if ya can't find it nowhere else, well, there it is.

PS -- the 'bay shows a UK seller offering fumaric @ $10/100g
« Last Edit: January 13, 2011, 05:02:49 AM by Vesp »
And the boy's father was shouting:

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"He doin' the stanky leg! He doin' the stanky leg! Two yearz ol' an' he doin' the stanky leg an' he NOT EVEN TRIPPIN'!!"

The infant was, in fact, doing 'the stanky leg.'

Believe me boy, I seen everything.

Vesp

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Re: Entropymancer and friends present : The FASA Method!
« Reply #3 on: January 13, 2011, 05:03:36 AM »
I had more of an interest in turning it into a more OTC thing from salts sold at grocery stores vs novelty places or online.
 
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overunity33

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Re: Entropymancer and friends present : The FASA Method!
« Reply #4 on: January 13, 2011, 06:18:45 PM »
Has anyone here tried neutralizing an aqueous dmt fumaric acid solution and crashing out the freebase directly in the aqueous solution?  Saw it done on dmt nexus I think but looks promising, no acetone needed.

GardensOfJoys

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Re: Entropymancer and friends present : The FASA Method!
« Reply #5 on: October 01, 2011, 05:19:11 PM »
Would one be able to employ the FASA method to convert 4-ACO-DMT freebase to fumarate? 

My gut assumes so, but the limits of my o-chem expertise and lack of a clearly documented procedure, specific to that material, forces me to proceed with well founded cautions.

All feedback is welcome and will be very much appreciated!

Thanks!
GOJ
« Last Edit: October 02, 2011, 12:39:08 AM by GardensOfJoys »

atara

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Re: Entropymancer and friends present : The FASA Method!
« Reply #6 on: October 04, 2011, 01:47:38 AM »
Malic acid converts to fumaric acid when heated to about 120-150 C for a few hours. Malic acid is available v. cheap and clean as a dietary supplement.

GardensOfJoys

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Re: Entropymancer and friends present : The FASA Method!
« Reply #7 on: October 04, 2011, 06:22:58 PM »
Thanks! ;)  I can source the fumaric acid at >99% for next to nothing, so no worries there!   And after raising my query to another, he was able advise with:

Quote
Well, a quick solubility test using 10mg of 4-aco-dmt fumarate proved to be 100% insoluble in acetone. So assuming the freebase form is soluble in acetone, I would assume mixing with a fumaric acid acetone solution should cause the freebase to precipitate to the fumaric salt the same way dmt would.

and so I feel quite confident that the FASA method would work just as well with the 4-aco-dmt freebase.  time will tell! :D

antibody2

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Re: Entropymancer and friends present : The FASA Method!
« Reply #8 on: October 04, 2011, 11:35:16 PM »
Has anyone here tried neutralizing an aqueous dmt fumaric acid solution and crashing out the freebase directly in the aqueous solution?  Saw it done on dmt nexus I think but looks promising, no acetone needed.

Yes, you can neutralize and basify the dmt in an aqueous solution, but you will still need a non polar solvent to extract it from that solution. If you are asking if you can do without the NP extraction, I've never left it long enough to see if it will settle out on its own. But I wouldn't reccommend doing that because you will have no way of removing the residual NaOH or whatever you used to base it.

DMT is hard enough on the lungs as it is.

« Last Edit: October 04, 2011, 11:42:56 PM by antibody2 »

antibody2

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Re: Entropymancer and friends present : The FASA Method!
« Reply #9 on: October 04, 2011, 11:36:58 PM »
Would one be able to employ the FASA method to convert 4-ACO-DMT freebase to fumarate? 

Yes there is no question that this can be done. Your 4-AcO-DMT freebase is soluble in acetone.

GardensOfJoys

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Re: Entropymancer and friends present : The FASA Method!
« Reply #10 on: October 06, 2011, 04:27:08 PM »
Thank you antibody2!  Now I just need to wait on my smiling postman to deliver!

Sol Invictus

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Re: Entropymancer and friends present : The FASA Method!
« Reply #11 on: October 07, 2011, 04:37:33 AM »
 This is all very interesting!   :)

 Has anyone verified that 4-subst.-DMT even forms a fumarate salt? I find this to be rather unlikely as psilocybin and friends are, to my understanding, zwitterions and as such do not form 'salts' per se. If you look at the synths for these sorts of compounds in Tihkal you'll see that this fact makes purification of said compounds rather tedious, as a standard a/b extraction cannot be employed, and the Kugel-Rohr must be utilized in almost every case. I have never seen or heard of a psilocin/psilocybin 'salt', and these zwitterions are very difficult to render into a stable crystalline powder. The result is typically a gummy goo or oil-- even a wax is hard to form. The only example I can think of is the acetate ester of psilocin, 4-AcO-DMT, which is a bit more stable than the other esters, however even this ester is prone to fairly rapid degradation if not kept cool, dry, airtight, and out of direct sunlight.

 Please correct me if I am wrong on any of this. I am curious to see if the compound in question will form some kind of a fumarate ester, but I am not sure this is possible. I imagine that the 'point' of this research is to see if this compound, like DMT, can be made into a pure and stable aqueous solution that can be administered parenternally via classic routes, but I would venture to guess that most esters of psilocin would hydrolyze back into the 4-hydroxy pretty quickly.

  --Sol


StonedOwlsley

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Re: Entropymancer and friends present : The FASA Method!
« Reply #12 on: October 08, 2011, 08:03:00 PM »
@agmotes165, Thanks for the advice! Seems like it might be a bit costly with the fumaric acid costing so much, but I just moved to a state in which Naphtha is illegal and of course who wants to fuck around with xylene in their kitchen, so I really appreciate this FASA tip. I want to see how far we can take this, let's use acetone for eeeeeeeverything! hmmmm.....FASA through a soxhlet!!!

antibody2

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Re: Entropymancer and friends present : The FASA Method!
« Reply #13 on: October 11, 2011, 04:14:43 PM »
Has anyone verified that 4-subst.-DMT even forms a fumarate salt?

4AcO-DMT is commercially available as a fumarate salt. Although Antibody has been informed that it will not form an HCl salt. Same with nn-DMT, it forms a fumarate salt no problem, but the HCl salt will not crystallize. Also 4AcO-DIPT can be converted to an HCl salt. Never tried the fumarate.

Fumaric acid is available from online spice/food stores very inexpensively

Sol Invictus

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Re: Entropymancer and friends present : The FASA Method!
« Reply #14 on: October 20, 2011, 10:03:47 AM »

 Thanks for clearing that up AB2. I would still be surprised if psilocin and/or psilocybin formed a stable fumarate salt, especially psilocin.