TEK Ethyl acetate approach [CIELO]

[shroombee]

...and world consumption of ethyl acetate is rising...

And stock up on cactus. Once this tek gets out there'll be a run on cactus chips.

Which is fine. I've felt for many years that mescaline is the psychedelic the world can most easily integrate into society. Although DMT, Psilocybin, LSD, Ayahuasca, et cetera are currently getting all the attention from the podcasters and youtubers. Mescaline is relatively unknown in those circles. I see it commonly referred to as Peyote and not well understood that it is found in more than just Peyote. If legal, I imagine it would be cost effective to synthesize?

Mescaline is more forgiving of dosage mistakes than other psychedelics. More self-guiding and less likely to induce bad trips. Eco-friendly where folks can take a dose on Saturday morning, have a 16 hour staycation instead of using limited resources to travel, relax on Sunday integrating how beautiful their lives are, then go back to work on Monday spreading smiles and good will.

Okay so now back to the experiments.

 

[Loveall]

...and world consumption of ethyl acetate is rising...

Indeed it is: TOTO88 | Situs Togel Terbesar dan Terpercaya

What would be the way to recycle ethyl acetate after using in this tek?
Would be washing with water and drying with something like CaCl enough?

More or less, although if you're using it for basified pulls it would be good to include a sodium bicarbonate wash to minimise the acidity. You could otherwise use anhydrous sodium carbonate (soda ash) for the drying stage, which as we know can be produced quite easily from sodium bicarbonate.

I guess if you had the capacity for distillation you wouldn't be asking, but distillation would be a good option if there was any sound reason to free it from non-volatile contaminants.

This is a great question. I've been wanting to test reusing the solvent. In addition to what is mentioned above also want to try de-acidify by simply adding lime, possibly with water (this way no new ingredients are needed if lime works).

 

[Loveall]

Regarding fast/slow pulls, I'm starting to see indications that fast pulls may be best. Product is whiter and yields are great. Updating the tek.

Earlier I mentioned some patience is good. I think that applied more to the lime paste, giving it enough time to react.

The faster pulls need to be filtered, but this easy to do and ethyl acetate runs fast through the filter. I use a metal screw cap to screw the filter directly on the jar mouth (see below). I also have a french press, that may work great like shroombee suggested. A few minutes per pull seems like enough time.

 

[shroombee]

Regarding fast/slow pulls, I'm starting to see indications that fast pulls may be best. Product is whiter and yields are great.

Are yields with faster pulls better than the slow pulls, or about the same? I have some cactus basing right now (getting a baseline on a 24 hour basing time). I'll run fast pulls on this one.

Earlier I mentioned some patience is good. I think that applied more to the lime paste, giving it enough time to react.

Now that it appears fast pulls give a whiter product and yields are fine, I think a followup test would be basing times: 1 hour, 24 hours, 48 hours, et cetera.

The faster pulls need to be filtered, but this easy to do and ethyl acetate runs fast through the filter. I use a metal screw cap to screw the filter directly on the jar mouth (see below). I also have a french press, that may work great like shroombee suggested. A few minutes per pull seems like enough time.

The french press seems the most convenient for decanting the solvent off the loose cactus.

For most general filtering, I use a metal coffee filter basket sitting inside a 1,000 ml beaker. And for something like pouring the xtals out of the jar, these paper coffee filters fit perfectly in the metal basket. Propping the beaker up at an angle on some post-it notes gives it enough angle so that the xtals all collect in the corner making it really easy to remove the xtals from the paper filter.

Depending on what I'm filtering, sometimes I just use the metal filter basket and I don't bother with the paper filter. Like if I wasn't using a french press, I could pour the ethyl acetate through the metal filter and any loose cactus would be caught by the basket. The basket is also easy to wash.

 

[Loveall]

I'm seeing slightly better yields with the faster pulls. Maybe allowing the paste to congeal does make it harder for the ethyl acetate to pull mescaline like you suggested shroombee.

It's not that huge of a difference, both ways work. After some practice though, I do think fast pulls are slightly better overall. At some point it becomes personal preference. If someone really hates filtering cacti (even though the solvent flows quickly and well), and doesn't care about the product being slightly tan instead of pure white, they can let the paste congeal and have long times between pulls.

The paste reaction time is good to look at. I think an hour is enough (since the last stops changing), but maybe I'm wrong. Experiments with the same cacti would tell us.

These are details though, at some point we start splitting hairs. What would be good to see is more replication and to know if this working well for other people with other cacti sources in general.

One thing I wanna do is a "speed run". 1h paste reaction, quick pulls (20min total), quick 10min salting and shaking (20mg/g of citric acid in ethyl acetate so no product ends up on the walls hopefully), and quick drying of the filtered crystals pressing the filter with paper towels (25min?). Could go from raw dry cacti to dry crystals in under two hours with good yields and purity. Faster than it takes to make a simple water tea (?). This is just for fun/personal challenge.

 

[shroombee]

The paste reaction time is good to look at. I think an hour is enough (since the last stops changing), but maybe I'm wrong. Experiments with the same cacti would tell us.

Recall that I noticed a 24 hour basing time seemed to require an extra pull versus 10 minute basing. I powdered 150 grams last night, intending to do three separate extractions of 50 grams each to make some of these comparisons with the same source material. Maybe 1 hour, 24 hours, 72 hours basing time, all with fast pulls?

These are details though, at some point we start splitting hairs.

I agree we are close to the point of diminishing returns. It always seems to be the common questions though - how long to base, how fast to pull, how many pulls, et cetera. And with this tek delivering repeatable results, we can run these tests and have definitive answers including the supporting data.

What would be good to see is more replication and to know if this working well for other people with other cacti sources in general.

I'm working with Peruvian Torch right now. I have another batch of Peruvian from a different part of the world, so to speak. Also San Pedro and Bridgesii. So I will shortly be running extractions on those. I'm wondering if another tek is better for Bridgesii to get more of a full spectrum extract. This would be my first experience with Bridgesii so I don't know what to expect.

One thing I wanna do is a "speed run". 1h paste reaction, quick pulls (20min total), quick 10min salting and shaking (20mg/g of citric acid in ethyl acetate so no product ends up on the walls hopefully), and quick drying of the filtered crystals pressing the filter with paper towels (25min?). Could go from raw dry cacti to dry crystals in under two hours with good yields and purity. Faster than it takes to make a simple water tea (?). This is just for fun/personal challenge.

Yes! I was thinking the same thing this morning. How fast can we run the process and still get the same results. To quick dry the xtals, maybe spread them into a thin layer on a baking dish. That's one thing I really like about working with ethyl acetate versus limonene: ethyl acetate evaporates quickly and cleanly. I feel like some of it dripping is less a mess than limonene. And cleanup is so much faster too.

To dissolve 20 mg/g citric quickly, I need to use a magnetic stirrer. I haven't seen 20 mg/g anhydrous grains of citric dissolve quickly without a lot of agitation. Or I may try salting with a solution of 50 mg/g saturated ethyl acetate (will increase overall extract volume by 11.1%).

BTW, having no product on the walls may be due to 10 minute agitation with the magnetic stirrer. It might not be due to the 20 mg/g citric. Or maybe it's a combination.

 

[metta-morpheus]

I now have a jar of around a quart of green cloudy ethyl acetate in the fridge. The only variant I had from the tek was I had to use a square casserole dish for the paste, as I just used the last of my quart jars on grain the other day. And I collected my pulls in a gallon pickle jar, so the xtals may be a little difficult to retrieve all the way in the bottom. The casserole dish worked well, in that it was very spread out, and I just had to jiggle the dish to get The solvent into the paste, tilt the dish, and it all collected in a corner. I 100% am getting a French press for this next time. When I went to squeeze the material in the end to get the last bit, the stuff presses even easier that coffee grounds. I will update later tonight or tomorrow morning, hopefully with news of crystals!

 

[shroombee]

I now have a jar of around a quart of green cloudy ethyl acetate in the fridge.

:thumb_up:

I collected my pulls in a gallon pickle jar, so the xtals may be a little difficult to retrieve all the way in the bottom.

After pouring the solvent and the loose xtals through a coffee filter, you can retrieve the rest out of your pickle jar by using some warm water and swirling it around. Evaporate the water in a dish. This might be obvious, but don't pour the water through the coffee filter holding your xtals because the water will dissolve xtals and they'll slip through the filter.

I will update later tonight or tomorrow morning, hopefully with news of crystals!

When using 5 mg of citric per gram of solvent or greater, and ensuring it all dissolves into the solvent, my xtals crash immediately. I'm conjecturing that all the yield is in that first few minutes, and there is no need to wait further or put the jar in the frig. I need to test this though.

 

[metta-morpheus]

Update: about an hour and a half later, I’ve added maybe another 2 g of citric and swirled over that time. It’s still cloudyish, in that it’s not a clear green, but it’s def not milky or to a point where things are crashing. More citric?

Also, I’m not sure if it was there from the start or not, as I just noticed it as I tilted the jar, but there is this tiny bubble of I’m assuming water that accumulates. Any thoughts? Could this have been water from pressing the material to hard, and squeezing out some water that goes past miscibility(?) with the ethyl acetate?

 

[Loveall]

Update: about an hour and a half later, I’ve added maybe another 2 g of citric and swirled over that time. It’s still cloudyish, in that it’s not a clear green, but it’s def not milky or to a point where things are crashing. More citric?

Also, I’m not sure if it was there from the start or not, as I just noticed it as I tilted the jar, but there is this tiny bubble of I’m assuming water that accumulates. Any thoughts? Could this have been water from pressing the material to hard, and squeezing out some water that goes past miscibility(?) with the ethyl acetate?

Hi, sorry it is not working right away.

Are there any xtals on the jar walls? If you shine a light trough the cloudiness, do you see glitter?

I don't know if you have water, I have not gotten those droplets, but haven't squeezed with ethyl acetate either. In the limo tek when I do squeeze I have let the limo sit for a day before salting and sometimes a tiny drops stick to the bottom of the jar (I just decant that).

Since you've already salted, if you do have water that is where the mescaline citrate could go. Was it cloudier earlier and clearing up without forming crystals?

One idea would be to add fresh ethyl acetate. It could absorb the water at 3.4% rate (assuming fresh = dry). So 100g of fresh ethyl acetate should absorb 3.4ml which is more than a few drops

How much citric acid have you added so far?

 

[metta-morpheus]

So your comment on the mesc being in that water droplet, the color of the droplet is incredibly milky.

So there seems to be a slight tiny bit of particulate in the solution. It’s hard to tell. I’ve added around 12 g of citrus at this point. Still just a tinted green solution. I will try the fresh ethyl to see if the water gets absorbed and anything in it can migrate to the ethyl to be crystalized.

 

[shroombee]

Update: about an hour and a half later, I’ve added maybe another 2 g of citric and swirled over that time. It’s still cloudyish, in that it’s not a clear green, but it’s def not milky or to a point where things are crashing. More citric?

I've added up to 20 mg citric per gram of solvent and I force it to dissolve quickly with magnetic stirring in 5-10 minutes (5 mg/g dissolves in about 2-3 minutes with magnetic stirring). I didn't get any xtals when letting the citric dissolve slowly over time, even when I added nearly 5 mg/g.

Solubility of citric acid monohydrate in ethyl acetate is ~53 mg/g, so be aware of that as you're adding citric.

The magnetic stirring might be a reason why I get crashing within a couple minutes. When I start stirring, I see the hard grains of citric acid swirling around the solvent and sliding along the bottom edge of the jar. Eventually there are less grains of citric but I see xtals swirling around. When I stop the magnetic stirring the xtals start falling to the bottom of the jar.

Also, I’m not sure if it was there from the start or not, as I just noticed it as I tilted the jar, but there is this tiny bubble of I’m assuming water that accumulates. Any thoughts? Could this have been water from pressing the material to hard, and squeezing out some water that goes past miscibility(?) with the ethyl acetate?

I don't squeeze the cactus, even at the last pull. Very little solvent is released by squeezing so I don't bother. I just manipulate the cactus very gently when adding fresh solvent. I don't even stir.

I've had water droplets appear in my jars that failed to crash. I pull the droplet out and let that evaporate on its own. Then I've had some success adding excess citric and using the magnetic stirrer. Yield was not as good as the jars in which I crashed the xtals immediately though.

So your [Loveall's] comment on the mesc being in that water droplet, the color of the droplet is incredibly milky.

This is interesting. The droplets I've seen in my failed jars were not milky, and neither did they contain much product after evaporation. If I saw a milky droplet in a jar I had recently salted, I would magnetic stir aggressively to get the water droplet to go back into solution. Or try Loveall's suggestion of adding some fresh ethyl acetate.

 

[Loveall]

shroombee's suggestion of agressively stirring makes sense (or alternatively shaking hard).

Hoping you get the milky/cloudy stuff to crash

 

[shroombee]

Intermediate observations with Run #4

Strategy: 24 hours basing, 3 minute timed pulls, total 6 pulls. Compare 5 mg/gram salting versus 15 mg/gram salting by combining pulls and splitting into two equal jars to be salted at 5 or 15 mg.

Only having 3 minutes between pulls to measure out fresh ethyl acetate, take notes, weigh recovery of previous pull, check pH strips, et cetera is difficult. Moving that fast can be error prone.
If I weren't taking notes and weighing everything accurately it would be easier.

I noticed the first two pulls were the same color pH paper. The 3rd pull was medium green. With Run #3, I did 10 minute pulls after 24 hours basing. And on that run the 3rd pull was a dark green, almost the same color as the first two pH strips. So I'm thinking the 3 minute pulls may be less effective. Next run I will go to 5 or maybe 10 minute pulls to test this.

Six pulls appears to be totally unnecessary based on the color of the pH paper for pulls #5 and #6, at least with this combination of basing and pull time. I don't know if leaving the last pull longer would grab more freebase.

For salting, jar (A) is 15 mg/gram and jar (B) is 5 mg/gram. Spun both for 10 minutes at the highest speed in which the liquid doesn't splash out of the jar.

Notes on Jar (A)
Wasn't paying that much attention to the early stages of spinning. Noticed some small xtals sticking to jar sides at 2 minutes into the spin. Stopped spinning at 5 minutes. Looked like all the citric dissolved. And there is a lot of xtal snow spinning around the solvent. It looks like there are no more clouds and the solvent would be clear after the snow settled. Spun the final 5 minutes to be sure there is no undissolved citric and everything has reacted. This extra 5 minutes is probably unnecessary.

Notes on Jar (B)
Watched this one more closely. Upon adding citric, the solvent is cloudy. I can see xtals within 30-45 seconds even in the cloudy solvent. Some sticking to the jar sides around 1 minute. These are larger xtals than jar (A). At 2:30 into mixing, the solvent is already clearer and I can now see the vortex in the center of the solvent. This may have been visible earlier, I wasn't looking for it. Stopped mixing at 5 minutes to check on things. Larger and more xtals sticking to the sides. Solvent appears clear with snow xtals spinning around. Spun the final 5 minutes to be consistent with jar (A).

During the last 5 minutes, I had an idea. I moved the jar around on the stirring pad so the spinning stirrer bar and the vortex would get close to the sides. That process knocked all the sticky xtals off the sides. I don't know whether that will eliminate having to use water to get xtals out of the jar. We'll see.

 

[Loveall]

That is very promising shroombee, and very similar to what I get. I've noticed too that if I shake continuously right after adding citric, fewer xtals get stuck to the jar walls, but I still get some.

Quick question, Did the paste consistency change as you pulled or did it stay loose/sandy?

I hope you get some nice white xtals on the rinsed filter and would love to see those pictures if you want to share (along with any xtals that you decide to slowly evaporate from water). I find that from ethyl acetate the xtals are small and with a fluffy or sandy. When those are dissolved in water and dried slowly at room temp (a few days) they become more compact, larger, and needle like.

Metta-Morpheus, any luck with stirring/shaking and/or absorbing potential water in the squeezed pulls with fresh ethyl acetate ?

 

[shroombee]

Quick question, Did the paste consistency change as you pulled or did it stay loose/sandy?

It stayed loose/sandy. In my lab notes I've described that texture as "crumbly". The total time from first adding ethyl acetate to decanting the last pull was 27 minutes. The cactus was still crumbly at 27 minutes.

After basing, I let the cactus sit for 24 hours in a sealed mason jar, then moved the cactus to a french press and broke it up with a fork. Then kept the cactus in the french press to do the 6 x 3 minute pulls. Very easy! I did press the cactus a little when decanting each pull to squeeze out another 5-10 grams of solvent. But I did not try to press it hard to force out solvent. Mixed very gently for no more than 30 seconds after adding fresh ethyl acetate for each new pull.

I hope you get some nice white xtals on the rinsed filter and would love to see those pictures if you want to share (along with any xtals that you decide to slowly evaporate from water).

Will do!

 

[metta-morpheus]

So more updates...

I added more ethyl. About 200 ml, small increments at a time. The blob got smaller, it never fully went away. But then I added 3 grams of citric, and shook. All of a sudden a bunch of crystal globs, some quite large, started swirling in the bottom. Solution is a translucent green now. I think I might add a dash more citric to see what happens. But I think other than that I’m ready to filter, dry, and weigh.

Edit: about an hour later, Something compelled me to touch the crystal goop while it’s drying, and lick my finger. Tastes very sour, just like citric acid. I’ve ran fresh ethyl over the filter 3 times, and a fourth after tasting it.

 

[downwardsfromzero]

So far I've only been able to source butyl acetate otc and will do a few preliminary tests including checking if citric acid is sufficiently (or even remotely :roll: ) soluble in BuOAc before attempting anything with this variation.

Here is a comparison of some selected physical properties for the two solvents:

EtOAc vs. BuOAc
logP 0.73 vs. 1.8

viscosity 0.423 vs. 0.685 (mPa.s @ 25°C)

surface tension 24 vs. 14.5 (mN/m @ 20°C/25°C)

Butyl acetate is less polar, obviously. I would anticipate this would lead to more impurities being pulled from cactus material so I might just have to be patient and hold out for some EtOAc.

fwiw, We can see that buffered, wet butyl acetate has been used to recover mescaline in modest yield from simulated post-mortem liver tissue: Redirecting
and BuOAc/CHCl3 was used to develop TLC of dansylated Pelecyphora aselliformis alkaloids including (N-dansylated) mescaline: https://doi.org/10.1126/science.176.4039.1131

 

[Loveall]

So more updates...

I added more ethyl. About 200 ml, small increments at a time. The blob got smaller, it never fully went away. But then I added 3 grams of citric, and shook. All of a sudden a bunch of crystal globs, some quite large, started swirling in the bottom. Solution is a translucent green now. I think I might add a dash more citric to see what happens. But I think other than that I’m ready to filter, dry, and weigh.

Edit: about an hour later, Something compelled me to touch the crystal goop while it’s drying, and lick my finger. Tastes very sour, just like citric acid. I’ve ran fresh ethyl over the filter 3 times, and a fourth after tasting it.

I think this is great news, welcome to the snow globe party . If you are still tasting citric it should wash away with fresh ethyl acetate. Did you get a ring of green on the filter? Are the xtals white? They should not be goopy, once dry the should be xtaline, with a fluffy to sandy texture. What about the jar walls, are they coated with xtals?

Mescaline citrate has some bitterness but not a lot. Maybe some hints of sourness too, IDK my taste buds are subjective. The MS and bioassay indicate it is pretty pure/potent, despite the mild bitterness. It is a lot less bitter than a raw alcohol resin and I think more mild than mescaline sulfate (again, subjective). I imagine some traces of citric could affect the flavor since citric is very sour and will quickly lower pH. When dissolved in Kombucha I could barely notice 500mg of what I think is mescaline citrate from this process according to Benz's MS analysis.

I wonder how you got what we think is water drops. I have not had this issue, but have not squeezed much other than with the flat part of a butter knife. It is possible to dry Ethyl-acetate with CaCl2 or MgSO4 or Na2SO4, or Na2CO3, or K2CO3 (I've tested all and prefer CaCl2 as it is less messy and easier to decant) before salting. We removed this drying step since it didn't seem to help with anything (no yield or apparent purity boost), and depending on the drying agent used it was hard to filter, but maybe it could have helped in your case.

One question is, were your pulls in a warm environment? It could be that water solubility in ethyl acetate decreases with temperate, and if the delta between room and fridge is high then water drops can form. If this continues to be an issue maybe settling in the fridge and decanting any drops that form before salting would help out. However, there should be a water buffer, because when pulling from an alkaline water, ethyl acetate should absorb less than 3.4% water. Perhaps waiting a few minutes before decanting helps to reach equilibrium with the alkaline paste and reduces the water below 3.4% a bit. Also, since citric acid is soluble in both water and ethyl acetate, adding it may also help the two be more miscible and that may have helped in your example.

It sounds like 3 people are getting xtalization, and shroombee and I are both getting multiple repeats. I've also had 3 friends try this product (after the MS results) and all had a good experience and no stomach discomfort. Shall we move the tek over to the main wiki? Current iterations has:

-1 hour or more of paste reaction with lime (shroombee has the highest yields and did 24 hours but we don't know if his cactus is just better)
- 4 total pulls of a few minutes each with minimal stirring for the first few seconds (shroombee and I are both seeing that 4 pulls seem enough)
- 5mg/g (~0.5%) citric acid salting to force xtalization with shaking or stirring. Should we increase this? Seems that higher is more robust to forcing xtalization and shroombee has tested up to 2% without issues (~5% carpet bombing should be theoretically possible), but there will be more traces of citric. However, any lingering excess citric after filtering should be taken care of with extra rinses.

I think we are in pretty good shape. Let's see what happens to Metta-Morpheus xtals and if all looks good there I propose we publish the new TEK on our wiki. If we do find that longer paste reaction time is indeed better or that there is a better way to pull we can always update those details later.

 

[metta-morpheus]

So I’m not fully confident in my results. Maybe it’s not fully dry yet. But I have a final weight if 1.29 grams off 100 gram cactus(Pretty high) and these crystals are very sticky. I can mold them into a ball, and my fingers are slightly sticky after doing so.

Flavor is a little more bitter than earlier, but still a sour forefront. They are slightly off white in color.

If I were to do a bio assay, it would be safe to assume that at worst case I’m eating a big ball of citric acid right?

Also, the filter has an oily stain leftover where the crystals were collected. Attached is pic.