Discussing Alternative Spice Extraction Techniques

[Infundibulum]

Hi all,

SWIM has made some interesting observations lately regarding the solubility of dmt fumarate in acetone (basically it is totally insoluble) and this initiated some nice discussions with 69ron on the Pure DMT Fumarate from freebase DMT topic, which led to the consensus that other extraction teks can be developed using less toxic materials and abolishing (or minimising) the use of non-polar solvents.

The different theoretical teks proposed so far are:

1 - Mix powder mimosa with 1 part calcium hydroxide.
2 - Add enough water to make it wet and mix. It should be like wet clay. (This freebases the DMT)
3 - Spread it out and let it dry completely.
4 - Dissolve it in acetone and filter out the solids. (Freebase DMT and other junk dissolves into the acetone)
5 - Saturate the acetone with fumaric acid.
6 - DMT fumarate precipitates out of the acetone. (Some other junk might also precipitate out the first time)
7 - Mix DMT fumarate with 1 part calcium hydroxide.
8 - Add enough water to make it wet and mix. (Freebase the DMT again)
9 - Spread it out and let it dry completely.
10- Dissolve it in acetone and filter out the solids. (At this point only alkaloids like DMT should dissolve)
11- Evaporate the acetone to get nearly pure freebase DMT.

and

1) acid extraction of MHRB. Your acid is FUMARIC ACID, so you convert all dmt to fumarate salt
2) boil down the extracts to a very very low volume.
3) add excess of acetone and cause precipitation of fumaric acid and DMT fumarate
4) collect precipitate and freebase it

Or:

1) extract MHRB with acetone and filter off all pieces. (soxhlet should work miracles here)
2) (optional)evap to a managable volume.
3) add excess fumaric acid.
4) see the beautiful precipitate falling.
5) freebase it

The idea of this topic is therefore to gather individuals' observations, ideas and propositions so that other experimenters can read them, comment on them or avoid doing them if negative feedback from other people is given.


SWIM's latest observations regard:

A) The formation of fumarate salt of the other MHRB alkaloids aka jungle spice;
SWIM did a STB on MHRB, pulled with naptha + collected the dmt, then did 3 xylene pulls which were evaporated down to a thick oil with strong indole smell. SWIM couldn't wait for the ages it usually takes for this oil to get solid; SWIM mixed this oil with fumaric-acid saturated acetone (FASA) and converted all of the alkaloids to the fumarate salt which quickly precipitated, leaving behind an acetone containing lipid impurities. When the latter acetone was evaporated, a yellowish lipid layer was left with no indolic smell. SWIM thinks to try snorting the jungle spice fumarate as well as freebasing it.

B) FASA was added in both naptha and xylene pulls from Diplopterys cabrerana after A/B extraction causing the salted alkaloids to precipitate. FASA was added until no more precipitation formed. Precipitates were collected and naptha and xylene containing FASA were washed in excess water to remove the residual fumaric acid and most of the acetone and were re-used for further pulls. Now SWIM uses the same ~100ml of non-polar solvent again and again until no further fumarate salts precipitate after FASA addition.

Now SWIM plans to freebase the fumarate salts in the following way:
1) dissolve them in the minimum amount of water possible
2) dropwise add water saturated with sodium carbonate so that freebases precipitate
3) collect the freebase precipitates


Any ideas / suggestions are only helpful!

 

[fourthripley]

I think Noman tried an acetone extraction of mhrb with no results. 'Well that didn't work a shit' is the thread/post.

 

[Noman]

I think Noman tried an acetone extraction of mhrb with no results. 'Well that didn't work a shit' is the thread/post.

That was an extrraction from straight bark - not bark treated with calcium hydroxide.

This all looks promising, looks like my friend has a lot of work ahead.

 

[69ron]

I think Noman tried an acetone extraction of mhrb with no results. 'Well that didn't work a shit' is the thread/post.

That was an extrraction from straight bark - not bark treated with calcium hydroxide.

This all looks promising, looks like my friend has a lot of work ahead.

SWIM also tried an acetone extraction from straight untreated bark and it didn’t work. That's because the DMT is in some salt form in the bark that’s nearly insoluble in acetone. Freebase DMT is highly soluble in acetone. If the DMT was in freebase form in the bark, then a straight acetone extraction would work very well. A straight naphtha extraction of untreated bark will also not work (that’s why the STB tech uses sodium hydroxide). Nor will a DCM extraction. The DMT needs to be freebased first, and then it can be extracted with acetone, naphtha, DCM, etc. That’s why that method above treats the bark with base first. It’s based on a Yopo/Vilca extraction that works quite well for Yopo/Vilca.

 

[69ron]

SWIM did the following and made a discovery that led him to start working on a salting out tech for mimosa (which he hasn’t completed yet):

1 Soxhlet extract 100 grams of mimosa with 700 ml 91% IPA and 10 ml 30% HCl solution for 10 hours.
2 Filter IPA.
3 Boil down to 25-50 ml.
4 Add 450 ml water.
5 Add 35 grams of salt and mix well.
6 Filter out the precipitates containing DMT HCl and some other gunk.

Believe it or not, DMT HCl actually precipitated out of the solution, along with a bunch of other gunk. The yield was low, but the bark may have been bad quality bark. SWIM then did an A/B on the gunk and recovered about 0.1% DMT from the bark. Not bad, but not great either.

DMT HCl is apparently very poorly soluble in brine. This is similar to harmine HCl and harmaline HCl.

This was discovered by accident. SWIM was attempting to do a salting out of the DMT during the freebase extraction step by adding sodium carbonate to a brine solution of DMT HCl, and discovered the DMT HCl actually came out during the acid part of the extraction just like harmine HCl and harmaline HCl do.

What to do from here? SWIM’s lab is under construction and he can’t continue his tests for a while.

 

[Infundibulum]

SWIM's FOAF posted this on Drugs forum, but it was intended for the Nexus, which, at this time was down without any hopes for resurrection:

Hi all,

SWIM's FOAF would like to share his experimental observations on novel ways of spice acquisition. In a way it is a follow-up from the ceased dmt-nexus forum where similar discussions were held. SWIM's FOAF has been able to extract dmt from MHRB using just water, acetone, citric acid, fumaric acid and sodium carbonate. The purpose of sharing such experimental results is immensely useful because they can build platforms onto which others may be able to add ideas and (hopefully!) resulting in faster, more efficient, more clean, and more eco-friendly teks.

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.

Control: If no fumaric-acid saturated acetone is added in the citric-acid saturated acetone extract (step 4) NO precipitates are seen after 3-4 days. This suggests that the precipitates are the fumarate salt of "some kind" of alkaloid.

Considerations:

1) In a pilot experiment of SWIM's FOAF just acetone was ued for the initial MHRB extraction. Addition of fumaric acid saturated acetone did not produce any precipitates immediately and on the other hand this silly guy did not wait for few days to see if anything precipitates.

2) Step 7 can be tricky. Sane humans would most likely go for an already tested A/B extraction using small quantities of a NP solvent.

3) this method definitely takes ages; it relies on the acetone insolubility of the alkaloids' fumarate salts. The rate limiting step is the conversion of alkaloid-citrate to alkaloid-fumarate. This problem could be overcome IF one was using an acid weaker than fumaric acid. This acid must be available in relatively anhydrous form (like the case of citrc and fumaric acids) and must be dissolvable in acetone. A good candidate could be glacial acetic acid (=100% acetic acid) since it has a pKa of 4.75 and is therefore weaker than fumaric acid. But not everybody can get glacial acetic acid easily (as opposed to teh other chemicals used in this method).....

Any suggestions / corrections and improvements are more than welcome!

 

[amor_fati]

{moved this from the fumarate thread}

SWIM is planning to experiment with freebasing by this method:

7 - Mix DMT fumarate with 1 part calcium hydroxide.
8 - Add enough water to make it wet and mix. (Freebase the DMT again)
9 - Spread it out and let it dry completely.
10- Dissolve it in acetone and filter out the solids. (At this point only alkaloids like DMT should dissolve)
11- Evaporate the acetone to get nearly pure freebase DMT.

SWIM didn't really notice the potential genius of this 'til SWIM started reading up on anadenanthera seed extraction. Has anyone tried this yet? What would be the best way to filter out the solids? SWIM is relatively inexperienced with acetone. Is there a safe way to speed up the drying process of the aqueous phase? Dessicant? Light heat application? What quality of crystals result from evapping acetone?

 

[69ron]

For Anadenanthera seeds, where the main thing you're extracting is freebase bufotenine, heat is fine. Freebase bufotenine can withstand very high temperatures before boiling away. It boils at 320 C (608 F).

For freebase DMT, heat is not good. It boils away at 60 C (140 F) and above. To speed up the process desiccants can be used instead of heat.

Actually, salt can be used as a cheap desiccant in this case because salt is insoluble in acetone. If you dump a bunch of salt on the water, it will form a gel like salty material that's insoluble in acetone, and then you should be able to extract the DMT with acetone. This works because water's attraction for salt is higher than water's attraction for acetone. Salt also raises the polarity of the water and that also makes both DMT and acetone less soluble in it. SWIM has tried that before and it definitely works. You must use a lot of salt. You need to reach the oversaturated point for it to work really well. For example, for 100 ml of water you’d add 100 grams of salt. Salt is CHEAP. 100 grams of pure table salt costs about $0.22.

 

[amor_fati]

Thanks for the advice!

SWIM attempted a modified version of the method stated above: An unmeasured but identifiable amount of jungle-spice salt was combined with an excess of sodium-carbonate. Water was added to the mixture until thoroughly wet. The mixture was stirred periodically. Salt was added until excess water was absorbed and allowed to absorb completely until dry. Acetone was added and the mixture was stirred. Acetone was filtered, collected, and poured into an evaporation dish.

After a few hours, the acetone had evaporated and left oily deposits that smelled of DMT. After being left overnight, the oil deposits had dried leaving waxy residue. A significant amount of the residue could be scraped and collected, and the rest was dissolved into toulene (to be salted out later). The yield appeared to be what was expected.

SWIM believes that the success of this method used for jungle-spice could be visually gauged because of it's dark color. However, pure spice wouldn't be so easily gauged, and would require measurement to determine whether it would work using this method. Judging by the apparent successes of basifying MHRB alkaloids with sodium carbonate, the method should prove successful.

SWIM's next experiment with this method will be scaled up and measured but will again utilize jungle-spice. The yield will then be tested for activity, though SWIM has next to no experience smoking jungle-spice.

 

[amor_fati]

350mg of jungle-spice fumarate was mixed with 2g sodium carbonate. Aprx. 5-10mL distilled water was added and the mixture was stirred until all jungle-spice was thoroughly melted. The mixture was allowed to sit for aprx. 1hr. Non-iodized salt was added until all water was absorbed; the total volume of the mixture was 15-20mL. The mixture was allowed to sit overnight. Acetone was added until total volume reached 50mL, and the mixture was stirred until no brown jungle-spice oils could be seen. The acetone was decanted into an evaporation dish.

(SWIM believes that the amount of sodium carbonate could be reduced to about 1g, judging by the sizable rock of it that wouldn't dissolve. Perhaps staying just above 2:1 would be ideal.)

The resulting acetone had a brownish hue. A yield of ~230mg freebase is expected. Evaporation results to follow soon.

 

[513orangejuice]

Wont sodium carbonate make about a carbon dioxide? from householdproducts.nlm

"Super Washing Soda will react with acids to yield carbon dioxide gas which can accumulate in confined spaces. Do not enter confined spaces until they have been well ventilated and carbon dioxide levels have been determined to be safe."

link:

http://householdproducts.nlm.nih.gov/cgi-bin/household/brands?tbl=brands&id=3005022

??? how much does it make? is it safe?

 

[fourthripley]

Co2 generated from sodium carbonate + acid won't be injurious to health, the main risk is that your solution will froth over and cause loss of product.

 

[513orangejuice]

oh, thank you. i see i was trippin now,, lol

 

[513orangejuice]

btw, this is a awesome thread. Cant wait to see the results!!!!

 

[amor_fati]

After the first acetone pull from the mixture, SWIM noticed that the little bit of acetone left in it had dried, leaving brown discoloration, signifying leftover spice. A second acetone wash was performed and combined with the first that was already about half-way evaporated, and this slowed down the process quite a bit.

A satisfying amount of crystals are forming from the oil deposits in the dish, which have nearly completely dried. SWIM believes that his acetone wasn't completely dry, and that this is slowing the process. The dry mixture still smells of DMT, so a third pull will be performed after the first pulls' yields are dried scraped and collected.

SWIM believes that the pull should be stirred more before decanting (SWIM only stirred for about 1 min).

 

[513orangejuice]

Sweet! What brand of acetone are you using? What brand of sodium carbonate you using bro? Arm and Hammer ?
Ive been wondering how good acetone would pull from a sod carb base mix,... So the spice was in salt form before you you based it, right? Bravo my man. Is there a reason for using 5-10mL distilled water ensted of acetone to make the base solution? I know a little normal dmt might be left over from fumaric - N - it up, but wouldnt dmt fumerates insolublity in acetone help the basing process if acetone was used in place of the h20? Not trying to act that i know anything about chemistry or nothing, actually i ask because i know NOTHING about chem, lol. Is it because introducing dmt fumerate salts with a sod carb/acetone mixture might cause some of the the salts to precipitate ensted of getting turned into dmt freebase?, cuz from what alot of posts SWIMs read, dmt fumerate can precipitate pretty quickly in acetone,...

 

[Infundibulum]

Awesome job amor-fati! SWIM's FOAF has also noticed (in slightly different experiments) that both sodium carbonate and sodium hydroxide can turn brownish after an acetone treatment. More precisely, when he was trying to freebase fumarate alkaloids he had dissolved them in water, then basified and finally wait few days for the freebase crystals to form in the basic solution. He then decanted the basic solution on top and let the freebase crystals to dry.

This resulted in a mixture of the freebase crystals, any residual sodium carbonate AND sodium fumarate! SWIM's FOAF then washed this residue with acetone to get the freebase out and noticed that the undissolved residue was of brownish nature. At this point he assumed that it could be 1) the sodium fumarate itself (unlike, since sodium fumarate is white)? 2) some impurity that was absorbed onto the sodium carbonate and sodium fumarate?

Who knows? but washing this brown residue with more amounts of acetone did not yield any more freebase, he therefore concluded that it might be some impurity that was captured. But the jury is still out there!

SWIY's case is similar; he mixed jungle-fumarate with sodium carbonate plus enough water to make a paste. The reactions going on here are:

1) Na2CO3 -> 2Na+ + CO3--, then CO3-- + 2H2O <-> H2CO3 + 2OH-

2) dmt-fumarate-dmt -> 2dmt+ + fumarate--, then dmt gets freebased due to the high pH (high OH-)

3) 2Na+ + fumarate -> sodium fumarate

All these processes depend on the presence of water. As long as SWIY lets the paste dry, he will be left with:

a) the freebase dmt
b) the unused sodium carbonate
c) the sodium fumarate.
d) the carbon dioxide that has left SWIY's paste and join the atmosphere (note that "H2CO3" in the first equation disintegrates to CO2 and H2O

Hope that helps!

 

[amor_fati]

Sweet! What brand of acetone are you using? What brand of sodium carbonate you using bro? Arm and Hammer ?
Ive been wondering how good acetone would pull from a sod carb base mix,... So the spice was in salt form before you you based it, right? Bravo my man. Is there a reason for using 5-10mL distilled water ensted of acetone to make the base solution?

SWIM's using arm & hammer and kleanstrip.

Na2CO3 is insoluble in acetone but soluble in water, just as the fumarate. Both need to be dissolved to facilitate reaction.

This resulted in a mixture of the freebase crystals, any residual sodium carbonate AND sodium fumarate! SWIM's FOAF then washed this residue with acetone to get the freebase out and noticed that the undissolved residue was of brownish nature. At this point he assumed that it could be 1) the sodium fumarate itself (unlike, since sodium fumarate is white)? 2) some impurity that was absorbed onto the sodium carbonate and sodium fumarate?

Who knows? but washing this brown residue with more amounts of acetone did not yield any more freebase, he therefore concluded that it might be some impurity that was captured. But the jury is still out there!

The sodium fumarate had completely slipped SWIM's mind! Though in SWIM's case, it seems to be a combination of that and leftover freebase, judging by the smell.

 

[513orangejuice]

OOHhhhh,.....im retarded, nevermind, lol

 

[amor_fati]

SWIM's final yield from the first two pulls is 168mg. This isn't the expected yield, but it's a high enough yield to perhaps validate the method. Any loss could be attributed to human-error. The third and final pull is on the evap dish, however, and may prove to make up for that missing 60mg (note that the residue leftover from the first evap has been allowed to dissolve into the third acetone pull). The crystals, once scraped, took on the expected waxy consistency and tan hue. Also note that there were still minor deposits of oil on the dish when scraped, so the crystals were scraped in such a way as to collect that oil; the crystals were reasonably dry by the end of this process.

The third pull seems to have been adequately thorough, as the completely dry leftover dry mixture from which the pull was performed, appears perfectly white and has only a very faint scent of DMT.


On a related note, a conversion of DMT-fumarate to freebase within a Na2CO3 solution, pulling with naphtha, yielded a dark crystalline mass floating atop the aqueous solution, not dissolving into the naphtha. SWIM first thought the mass to be emulsions, but then scooped them out and dried them. The whole mass is quite solid and has a crystalline sparkle. SWIM believes the dark mass to be jungle-spice, as the fumarate most certainly contained small amounts of jungle-fumarate.

Note that both solutions have been quite chilled. The naphtha is decanted, unsaturated, immediately after freeze-precip, into the basified solution, which is being stored in a chilly area. It is shaken thoroughly to mix, then left to separate in this chilly area.

The naphtha itself has been consistently saturated on every pull thus far, but SWIM has yet to attempt another pull without the presence of this dark mass in the solution.

Thoughts?