32 replies to this topic

[Norman]

So, having some free time and a couple of root barks at hand I find myself contemplating the drytek.
Materials such as lye and decent fast evaporating NP solvents are getting harder for some people to find, and in keeping with the “for the masses” spirit I want to come up with something using super commonly available materials. I’d also like it to be so easy that it wouldn’t be too much of a hassle to do on plants suspected but not proven to contain DMT since I’m starting to think that a large swath of the legume family might be viable candidates.
Here’s what I’m thinking -
Powder or grind the plant material and add just enough distilled white vinegar to wet it and add enough water to make it soupy.
Let it sit overnight - maybe in a warm oven or crockpot? I’m torn here because I’m thinking the heat will speed the reaction as well as drive off some of the excess acetic acid but I want this to be simple.
Add a weight equal to that of the plant material of calcium hydroxide or sodium carbonate. CaOH is what’s usually used and it’s what I’ve used in cebil dryteks, but NaCO would be even more commonly available even if one needed to make it from baking soda, I’m just not sure if it’s basic enough. (On a side note, what would even happen if you used ammonia here? The next step is to dry everything down, so would the alks just convert back into whatever salt when the ammonia evaporates?)
Dry down and pulverize.
To extract, I’m considering a couple of things.
Acetone is the tried and true choice and I suppose MEK would perform about the same. The alcohols could be tried - assuming people can get 99% IPA, methanol in the form of yellow bottle HEET gas treatment, or clean burning ethanol camp stove fuel. Any ideas on solubilities here would be most welcome.
I’m also thinking about canola oil since it’s super available and beyond suspicion like baking soda. Somebody on here whose handle escapes me used it in an A/B and had good results. Speak up whoever you are! Of course this would require salting, which is a royal pain in the ass.
Lastly what about butane? Like a honey oil extraction? Very cool and very easy if it worked.
Also thinking that some element of the FASA method might plug in here somewhere.
What do you guys think?

[Phineas_Carmichael]

We worked on this a little bit almost a decade ago, treating MHRB as one would cactus in a classic drytek, but lye and solvents and great MHRB were all mostly easily available at the time so nothing ever really came of it...

https://mycotopia.ne...tek-experiment/

 

So, having some free time and a couple of root barks at hand I find myself contemplating the drytek.
Materials such as lye and decent fast evaporating NP solvents are getting harder for some people to find, and in keeping with the “for the masses” spirit I want to come up with something using super commonly available materials. I’d also like it to be so easy that it wouldn’t be too much of a hassle to do on plants suspected but not proven to contain DMT since I’m starting to think that a large swath of the legume family might be viable candidates.

I really like the idea of a "quick and dirty" test extraction for suspect plants. There's a reason Shulgin titled that chapter in TiHKaL "DMT is Everywhere."

 

Here’s what I’m thinking -
Powder or grind the plant material and add just enough distilled white vinegar to wet it and add enough water to make it soupy.
Let it sit overnight - maybe in a warm oven or crockpot? I’m torn here because I’m thinking the heat will speed the reaction as well as drive off some of the excess acetic acid but I want this to be simple.

 

I've always been troubled by the acid step in dryteks. Is it there to force all the target molecule into a specific salt (instead of whatever natural salts are present in the plant) that more readily reacts with the base added in the next step? Without the defat that a standard A/B allows, I can't quite wrap my head around acidifying the plant source, only to basify it immediately. It just feels like an STB with an extra step. If the acid and some heat get everything into solution quickly without the long soak required in an STB, then I get it.

 

I think I just talked myself into getting it...

Add a weight equal to that of the plant material of calcium hydroxide or sodium carbonate. CaOH is what’s usually used and it’s what I’ve used in cebil dryteks, but NaCO would be even more commonly available even if one needed to make it from baking soda, I’m just not sure if it’s basic enough. (On a side note, what would even happen if you used ammonia here? The next step is to dry everything down, so would the alks just convert back into whatever salt when the ammonia evaporates?)
Dry down and pulverize.

Calcium Hydroxide isn't very soluble in water, and can cause problems later on, depending on the extraction solvent. Defiance mentions it at the very end of the thread I linked earlier. Sodium Carbonate can get your pH up to around 11 or so, so it should work just fine.

 

Ammonia will neutralize the excess acetic acid to form ammonium acetate, which is a hygroscopic white solid. This would probably make it difficult to dry down the mixture as it will absorb water from the air. The carbonate neutralizes the acetic into sodium acetate, which is not hygroscopic but does very interesting things in supersaturated solutions.

 

The drying down would also have to be performed without heat to avoid destroying the target. In the chemistry lab we would do this in a vacuum filter, pulling air through the filter cake until it was completely dry. I'm not sure the best way to do this in the "for the masses" clandestine lab. Filtering as well as possible and spreading out the paste to air dry over time might invite mold or oxidation of the freebase if it takes too long.

 

To extract, I’m considering a couple of things.
Acetone is the tried and true choice and I suppose MEK would perform about the same. The alcohols could be tried - assuming people can get 99% IPA, methanol in the form of yellow bottle HEET gas treatment, or clean burning ethanol camp stove fuel. Any ideas on solubilities here would be most welcome.
I’m also thinking about canola oil since it’s super available and beyond suspicion like baking soda. Somebody on here whose handle escapes me used it in an A/B and had good results. Speak up whoever you are! Of course this would require salting, which is a royal pain in the ass.

Any of these solvents should work just fine for extraction. The Nexus lists it as highly soluble in all 3 alcohols and both ketones. Acetone, MEK, and methanol have the lower boiling points, so would evaporate quicker than the more complex alcohols, provided whatever solvent used was as close to anhydrous as possible. If nothing else, adding baked epsom salts to dry whatever solvent was used first and filtering them out would be an adequate workaround.

 

Lastly what about butane? Like a honey oil extraction? Very cool and very easy if it worked.
Also thinking that some element of the FASA method might plug in here somewhere.

I would think butane would work spectacularly; it's non polar & evaporates super-quick. Supercritical CO2 might work as well. I'd never recommend either to the everyman chemist, as I know a one-eyed everyman, but if done safely it'll be fine.

 

I can't speak to FASA, having only read about it in passing, never really looking deeply into it. Might be a good way to clean an impure product if recrystallization isn't an option.

What do you guys think?

I like it.  I like it a lot. Just to make sure I'm clear on what's happening chemically I have to write it out.

 

1. DMT containing plant matter is soaked (with or without heat) in an aqueous acidic solution until all the DMT is present in the water as a salt.
2. The mixture is basified with a weak base so that all the DMT is converted into freebase.
3. The water is evaporated, yielding a powder consisting of plant matter, acid-base neutralization salts, and freebase DMT.
   1. ​Could the water be filtered off and only the goo left in the filter (filtrand) be dried?
4. The powder is washed with a polar solvent in which the freebase is highly soluble.
5. The solvent is evaporated, yielding freebase DMT.
6. Potentially use FASA to clean up impure product.

 Please check my work.

Edited by Phineas_Carmichael, 15 January 2021 - 01:06 AM.

[Norman]

My that was some time ago!
Thanks for the link, I’d forgotten all about that.
I think acetone will be the way to go since carbonate seems to be somewhat soluble in alcohol. I’ll give both carbonate and calcium hydroxide a shot and see where it takes me.
This whole thing came to mind when I was making creme brûlée and filling my torch with butane but I think I’ll leave the butane out. Images of federal prison with one hand blown off come to mind

[Norman]

And yes your synopsis is basically what I’m talking about.
I was thinking FASA when I was thinking about canola oil because I hate salting so much (ever since my beer bottle and aquarium tubing HCl gas generator-another time federal prison came to mind) but there is no way to concentrate the alks in canola oil.
I wonder now though, if the fumaric acid were dissolved in the acetone, which would presumably disperse in the oil, would the alks then precipitate?

[Phineas_Carmichael]

My buddy who lost an eye to a bad BHO extraction & a friend from high school who lost a foot in a motorcycle accident always go to halloween parties dressed as pirates. I'm sure they wouldn't mind a 3rd to complete their trio, y'all would definitely win the prison costume contest!

 

I hadn't thought of the unreacted base's solubility in the extraction solvent, being so used to non-polar solvents. Great catch with the Ketones. Calcium hydroxide will get your pH about a point higher than sodium carbonate, but I expect both will be adequate for the task at hand.

 

Salting is such a pain in the ass, and those gassing contraptions are always so dangerous, not to mention giving me terrible visions of Auschwitz. I like the idea of salting with FASA, presumably the liquids would separate and DMT fumarate would form at the interface.  If they precipitate & settle they might clog your sep funnel though.

 

I have concerns about miscibility between canola oil & acetone and about the solubility of fumaric acid in canola oil though. Canola oil is about 60% oleic acid and 20% linoleic acid, both of which are miscible with acetone according to pubchem. Chances are acetone and canola will not separate if the fatty acids are existing as free chains. All is not lost if those acids are existing as triglycerides on a glycerin backbone. However, a few Masters theses I managed to dig up that weren't behind paywalls seem to indicate that triglycerides in general are slightly soluble in cold acetone and highly soluble in hot. There is a chance that keeping the solutions cold would encourage separation, but I'm not sure how this would affect the solubility of DMT in the FASA, probably negatively. Clearly some small scale acetone & canola oil separation experiments would be in order before trying to extract with canola & salt with FASA.

 

Pubchem says fumaric acid is "almost insoluble" in olive oil & cites Merck so you should be good to go there, you won't lose all your acid to the oil phase.

 

This is fun. Keep us posted when you get around to experimenting.

Edited by Phineas_Carmichael, 16 January 2021 - 12:58 AM.

[Norman]

Yes this is fun. Ten years on, these thought experiments are a lot more fun than siphoning pH 13.5 solutions and evaporating toluene. Hmmm thinking things through first - damn I’m getting old.
As far as using FASA on a canola oil pull - I’m not expecting the acetone to separate. I’m hoping that it will disperse through the oil and carry the fumaric acid with it to form an insoluble salt with the DMT which would then precipitate.
That speculation is based on nothing but thinking out loud about food safe and FASA and salting and blah blah but it would be a neat trick.

[bezevo]

there are lot interesting plants comming to light   needing research ..  this thread might help thanks Norman

 

bellow is thread on possible alternative plants like  (Delosperma cooperi/Ice PPlant ) . lespedeza-s ,many or 100's of acacias ,the leaves and bark are rumored as strong as  root bark , same with many mimosa ...and various grasses

 

 

https://mycotopia.ne...r/#entry1457936

Edited by bezevo, 16 January 2021 - 12:01 PM.

[Norman]

Yep thanks for the reminder that the whole point of this is to be streamlined so that people will actually do it. FASA gassing and salting are beside the point.
Suspected alkaloid containing plants can just be ground up - I don’t see a need to dry them first - acidulated, based, and pulled with acetone which is then evaporated. A whiff of the residue with a flame put to it will tell anyone that’s experienced DMT if the plant is worth further research. I’ll try to come up with an apparatus that makes this as quick and easy as possible.

Phin - I had the same questions as you regarding the necessity of the acid step. I’ve always gone STB with cebil and it worked fine. I only initially included it here because both treks on the Nexus use it and they’re by people I respect. I’ve since also come to the same “why not?” conclusion you have. It might help nudge the goods out into solution. I’ll likely end up trying both.
Another thought - could the acetone be added to the mix before it dries? Would the freebase be soluble in the resulting acetone/water mix? Could you then filter it and pull the water out with baked Epsom salts? An extra step but a time (and oxidation) saver by not having to wait for the mud to dry.

[Phineas_Carmichael]

Yes this is fun. Ten years on, these thought experiments are a lot more fun than siphoning pH 13.5 solutions and evaporating toluene. Hmmm thinking things through first - damn I’m getting old.
As far as using FASA on a canola oil pull - I’m not expecting the acetone to separate. I’m hoping that it will disperse through the oil and carry the fumaric acid with it to form an insoluble salt with the DMT which would then precipitate.
That speculation is based on nothing but thinking out loud about food safe and FASA and salting and blah blah but it would be a neat trick.

Oh, precip the salts right out of the oil, that would be a neat trick! It will be a bugger to clean up, probably have to filter (and filtering cooking oil does not sound like a good time) then wash with a non-polar that would dissolve the oil but not the salts or something like that...

 

Fumaric is (probably) insoluble in canola, but with the acid already broken down into ions in the acetone, I can see one of 2 things happening. Either all goes according to plan and DMT fumarate crystallizes and crashes out, or the fumarate^- and H⁺ ions just recombine to form fumaric acid again and it crashes out. Worst case scenario, a combination of the two happens and you're left with a mixture of fumaric acid and DMT fumarate.

 

But you're right, this line of thinking is unnecessarily complicated. Perhaps we should dial in a simple method and tweak it later...

 

Phin - I had the same questions as you regarding the necessity of the acid step. I’ve always gone STB with cebil and it worked fine. I only initially included it here because both treks on the Nexus use it and they’re by people I respect. I’ve since also come to the same “why not?” conclusion you have. It might help nudge the goods out into solution. I’ll likely end up trying both.

I've been thinking a lot about that acid step and have decided it's definitely there to avoid the long soak times in traditional STBs. That acid and a little heat are going to break down polymers like lignin in the cell walls to get at the gooey DMT center a lot faster than alkaline solution will, especially with weak bases like we're talking here that can only get the pH up around 11 or 12. It's probably a necessary step to potentially make this a weekend project instead of a "stash-it-under-the-sink" project.

 

Another thought - could the acetone be added to the mix before it dries? Would the freebase be soluble in the resulting acetone/water mix? Could you then filter it and pull the water out with baked Epsom salts? An extra step but a time (and oxidation) saver by not having to wait for the mud to dry.

Any water in the acetone is going to adversely affect the solubility of DMT and introduce water soluble impurities (like the acid-base neutralization salts) into the final product, not to mention taking much longer than acetone to evaporate, likely producing a goo for a final product. If the aim is to check a suspect plant for DMT this is a fine result, G-d knows I've smoked more than my fair share of strange oils and waxes and had a lot of fun doing it! It's possible that drying the extraction solvent with epsom salts after the fact would suck out all the water, leaving the a/b neutralization products to precipitate out and be filtered along with the epsom salts, I'm just not sure how much water they can pull out. I've only ever seen them used to turn 90+% polar solvents anhydrous or remove atmospheric water absorbed by old solvent.

 

If the aim is to produce a crystalline-ish product, that mud needs to be as dry as possible, and I've been pondering that a bit today. Like I said before, in the chem lab we would use half an hour of vacuum filtration, break up that filter cake, and gently press it between successive layers of clean filter paper until no more water came out. A double-thickness of cone #4 coffee filters can sometimes be an acceptable substitute for lab-grade filter paper.

 

I was also thinking about labneh today. If you put yogurt in 6 or 8 layers of cheesecloth (or in a clean pillowcase) and hang it in the fridge over a bowl for a day or 3 a whole lot of whey comes out and you're left with a delicious (after you add some salt) paste almost like neufchâtel or cream cheese. Depending on the consistency of the mud after basification I bet you could give it the same treatment. It would remain wet enough to avoid oxidation, and cool enough to avoid mold, and might just be a good starting point for spreading thin to air dry for another little bit of time. After scraping up I think it could be crumbly enough to gently press between coffee filters to get it pretty dang dry.

 

Just spitballing, though. If creme brûlée got the whole thing started, maybe yogurt cheese can finish it...

Edited by Phineas_Carmichael, 17 January 2021 - 01:46 AM.

[Norman]

Okay here we go -
50g MHRB mixed with 100 ml vinegar/water diluted 1/3.
I’ll let that go overnight and then divide it and treat half with 25g calcium hydroxide and half with 25g sodium carbonate. Let that dry and extract with acetone.

I’ll go one better on the labneh method. I own a cheese press. Should be a part of any orgo kit.

[Norman]

Over a week on and both mixtures are still slightly damp. Credit that to my being cheap and only running heat in the bedroom all winter. 

After the vinegar water soak I divided the mixture in half and mixed one with 25g NaCO and the other with 25g CaOH. The NaCO mixture was a perfect mud consistency but the CaOH soaked up more liquid and I had to add 10ml of water to get the same consistency. The NaCO mixture turned a dark grey purple familiar to anyone who has extracted MHRB and the CaOH turned an orange brown - pretty much the same color as The Thing from The Fantastic Four. Both mixtures smelled of alkali and indole. Despite having an extra 10ml of water added, the CaOH mixture is the drier of the two. I guess the NaCO is somewhat hygroscopic?

They're both almost dry so I'm thinking of chancing a final drying in an extremely low oven to drive off the rest of the water so that I can do the extraction this weekend. Seems a tossup between oxidation from a long drying time and potentially losing product from heat. Maybe next time I'll break out the cheese press.

 

[bezevo]

So any UPDATES ?  Norman and Phineas_Carmichael....Lots of interesting possible plants ,trees , grasses  and alternative mimosas and  acacias out there that seem umm interesting possibilitys . hummm...

 

BEZ

Edited by bezevo, 17 February 2021 - 02:02 PM.

[Norman]

Sorry folks - laziness.

Everything has dried down, the CaOH was hard as a rock as expected. NaCO was more powdery. Both were pulverized in a mortar and 150ml of acetone was added and allowed to sit with occasional stirring. Mixture was squeezed through a cloth and rewetted with acetone and squeezed again. Acetone is now sitting in jars and will be decanted filtered and evaporated as soon as I get off my ass.

Even through the acetone fumes I can distinctly smell insole so fingers crossed.

[Norman]

And two months later here’s my “quick tek”.
Ha!
Sorry, honestly someone less lazy busy and devoted to cannabis than I could pull this off in a couple of days with the vast majority of that being hands off drying time.
So to recap, two batches of 25g powdered MHRB was mixed - one with 25g NaCO and one with 25g CaOH. Water was added to each to make mud and this was allowed to dry and powdered. Each was extracted twice with 100ml acetone which was run through a coffee filter and evaporated.
Both extractions yielded a really pretty orange red sticky oil that smelled like flowers and from initial whiff tests seems to be extremely active. Probably the most full spectrum MHRB extract I’ve seen.
Yield was .27g for the CaOH extract and ..35g for the NaCO, so just over 1% and under 1.5% respectively. Of course this is far from refined product from bark known to yield 1% pure white and another percent or so of dark so yields could be better but I’m sure they would be with a more pains taking technique.
The good news is that it’s a quick (other than the drying time) set it and forget it way to see if an unknown plant is worth exploring and it only uses readily available materials. I was happy that the NaCO actually worked better than the CaOH since it’s super available by heating baking soda. Now to see if alcohol works as well and maybe we’ll have a ban proof grocery store tek.
Coming up, I’ll try that as well as a FASA precip and on ACRB and desmanthus. Haha! See ya in six months!

[Phineas_Carmichael]

Hell yes!  Thank you Norman for keeping on this!!!

 

Ii'm super-glad that the sodium carbonate worked so well.

 

I can see this as a great way to quick-and-dirty extract a legume just to see what happens.

 

I can also see this as a large-scale extraction on known low-yield plants like phalaris grass.  The resulting full-spectrum goo could easily be treated to a standard A/B to yield crystalline product...

 

Thanks for all your hard work!

Edited by Phineas_Carmichael, 09 March 2021 - 02:41 AM.

[Norman]

Thanks Phin.

Yeah carbonate all the way.
More readily available.
Requires less water to hydrate so there’s less water to evaporate.
The dried product powders easily where the CaOH and plant mixture sets up like a brick.
When powdered it’s not as fine a CaOH so it doesn’t require as fine a filter.

I like to come up with a double ended system like an hourglass with the dry goods in the middle so the acetone can just dump back and forth.

That and the aforementioned cheese press to speed up drying.

[YoshiTrainer]

"extractions yielded a really pretty orange red sticky oil that smelled like flowers and from initial whiff tests seems to be extremely active."

So DMT smells like flowers?

[Norman]

To me it does. Especially rough extracts. The purer ones are more of a mothball/flower smell.
It’s an indole so that’s why.

[Phineas_Carmichael]

To me, all the tryptamines all have a delicious floral scent.

 

DMT smells very specifically like Catalpa flowers to me, so much so that walking by a flowering Catalpa tree is enough to practically give me a flashback...

 

*[A chemical from TiHKAL we don't talk about here]* smells like brand new sneakers or aquarium tubing to me, so much so that I avoid Foot Locker and pet stores when I'm at the mall...

 

Some of the other indole chemicals can smell like poop, but the chain on position 3 changes the smell...

........

 

I've been thinking a lot about the drying portion of this extraction and I'd like to think that pre-heating an oven to the lowest setting (usually around 170F ) and then turning it off before putting the spread-thin mud to dry overnight as the oven cools might not hurt the target molecule. 170F is well above the melting point of freebase DMT, but well below the boiling point I believe. 

 

I think that a speedy dry in the oven might not hurt things. At worst it might turn the freebase from solid to liquid and back again, much like we do with water when we make ice cubes...

Edited by Phineas_Carmichael, 13 March 2021 - 03:18 AM.

[pharmer]

our oven has a warming drawer that heats as low as 100 F       

 

if that helps anyone