TEK Ethyl acetate approach [CIELO]

[starbob]

I only put neutralized (and dried) EA back in the cans but i suppose i could have screwed up something. It had a dented corner I should've probably been wary of as well.

 

[Jan e Kharabat]

So Mescaline citrate can be salted out from Toluene by adding citric acid dissolved in acetone, but it's probably not a good idea to do so because then you cannot simply reuse the same toluene. I could've realized it before trying it out, but I am very confused these days and cannot figure out how to do even simple things... anyways, one issue is that the toluene/acetone mixture cannot be further used without getting rid of the acetone or without separating the two, I will keep the mixture until I get a distillation setup and will try to separate them.

The other problem is of the larger surface area and the fumes. That has been mainly the reason why I don't like dry teks, you have a bigger bowl with large open mouth, a whole lot of solvent just simply vanishes into the mixture and that... just gives me anxiety! and even if you are in a well ventilated space, you will still be close to the bowl, inhaling the toxic fumes. Heptane I can tolerate, but toluene is no fun! So... I think ethyl acetate is the best option for dry tek and toluene for A/B.

I will try the A/B method next and salt with benzoic acid. Would be great to know if someone knows about the bioavailability of the benzoate salt.

 

[doubledog]

Benzoate salt is easy to produce from toluene, and it makes nice crystals.

One member have reported interesting results here:

Ph will not go higher - Preparation - Welcome to the DMT-Nexus

 

[Twilight Person]

Already second extract failed might need some advice. I understand 2 factors are the most important to get the TEK working: 1. homogeneous powder / paste with correct consistency and 2. doing the fridge decant step carefully to not have too much or too less water for crystallization.

But already during trial 1 I decanted it after 24 h fridge and an expected amount of water was decanted. All fine, but then when adding citric acid (it also clouded as expected) there was no crystal growth. Instead just some slush at the bottom after 48 h. This was probably still water! Even though I did the fridge step correctly. All the mesc citrate was possibly in this was slush. Recovering it with some chemistry moves did mostly just made me losing all the rest ... poor cactus went into the drain basically.

Next trial I even turned my fridge from 8 °C to 4 °C. 24 h waiting, again decanted an expected amount of water. Added citric acid, it dissolved 100 % and clouded while doing so. But after 48 h again a water slush at the bottom. Maybe like 2-5 ml below 200 ml Ethyl Acetate. So where did that water suddenly come from? I did the fridge step reasonably. So no crystal growth because I think it is now all dissolved in that slush at the bottom. Now I did not already try recovering it from that. But remembering my last trial at this I dont have much hope that I will recover (most) of the mesc citrate here.

Because of this I am already scared to waste my cactus #3. So as I did all the steps according to the TEK I would ask the following:

What would happen if I completely DRY my EA? I mean yes, it is told a little water is good for crystallization. But as I wrote I already got this problem a second time. So I am tempted to just remove the water 100 % and then this can not happen. So what would happen if I do it? What should prevent me from doing so? I have not tried recovering #2 yet, but as my hopes are not too high I am already too afraid of wasting cactus #3. :thumb_dow




In case everything fails I would just extract with toluene and drop in benzoic acid. I guess here it cannot create the same issues, but I want to go the citric acid variant actually.

Thanks for any help and cheers!

 

[Quetzal7]

Already second extract failed might need some advice. I understand 2 factors are the most important to get the TEK working: 1. homogeneous powder / paste with correct consistency and 2. doing the fridge decant step carefully to not have too much or too less water for crystallization.

But already during trial 1 I decanted it after 24 h fridge and an expected amount of water was decanted. All fine, but then when adding citric acid (it also clouded as expected) there was no crystal growth. Instead just some slush at the bottom after 48 h. This was probably still water! Even though I did the fridge step correctly. All the mesc citrate was possibly in this was slush. Recovering it with some chemistry moves did mostly just made me losing all the rest ... poor cactus went into the drain basically.

Next trial I even turned my fridge from 8 °C to 4 °C. 24 h waiting, again decanted an expected amount of water. Added citric acid, it dissolved 100 % and clouded while doing so. But after 48 h again a water slush at the bottom. Maybe like 2-5 ml below 200 ml Ethyl Acetate. So where did that water suddenly come from? I did the fridge step reasonably. So no crystal growth because I think it is now all dissolved in that slush at the bottom. Now I did not already try recovering it from that. But remembering my last trial at this I dont have much hope that I will recover (most) of the mesc citrate here.

Because of this I am already scared to waste my cactus #3. So as I did all the steps according to the TEK I would ask the following:

What would happen if I completely DRY my EA? I mean yes, it is told a little water is good for crystallization. But as I wrote I already got this problem a second time. So I am tempted to just remove the water 100 % and then this can not happen. So what would happen if I do it? What should prevent me from doing so? I have not tried recovering #2 yet, but as my hopes are not too high I am already too afraid of wasting cactus #3. :thumb_dow




In case everything fails I would just extract with toluene and drop in benzoic acid. I guess here it cannot create the same issues, but I want to go the citric acid variant actually.

Thanks for any help and cheers!

I'm actually experiencing the same situation
First time, i recovered the water layer, based it with NAoH, pulled again with EA (100ml instead of the original 1000ml) and then i manage to get some crystals. So it might have to do with the concentration , and there's a kind of Offset - a minimal amount under which the concentration is too low to start the crystalisation process?
the 2nd time i tried, i got nothing at the end... maybe was a weak cactus ...

I think for my 3rd attempt, i'm gonna backsalt with vinegar and evaporate, so at least i know what's in there and if the cactus is yielding, and i can recrystalize in EA if i wish
any objection or disadvantage to that approach? does vinegar backsalting works the same with EA than D-limonene ?

 

[merkin]

Thanks! Has anyone tried mescaline benzoate? would it be suitable for ingestion?
I was thinking of a way to extract with toluene but make citrate, one idea I have is to dissolve citric acid in acetone and add that to the toluene. Acetone will dissolve in toluene, allowing citric acid to react with the freebase mescaline, mescaline citrate being insoluble in both acetone and toluene will crash out.

Hey Dasein, I have this topic on my mind atm but more regarding the benzoate than the citrate due to some remarks about its probable increased potency (by weight) beyond its HCl equivalence. But answer is yes, oetzi13 has tried ingesting m.benzoate and with very interesting results IMO

As doubledog suggested: check this thread out:

Curious to hear comments on it?

Benzoate salt is easy to produce from toluene, and it makes nice crystals.

Would you mind a bit of details on your 'tek' here please. I am very keen to try this and thanks for that pointer on the above thread. I find oetzi13's experience quite intriguing and would very much like to bio-assay myself.

 

[Twilight Person]

Anymore comments on what would be the downside of drying the EA? Like maybe not with a real drying agent, but mixing it with saturated NaCl solution and then separating layers again. Would not remove 100 % of water, but way more than the fridge step. What is then the downside of removing "too much water" from the EA prior to crystallization?

Cheeerss!

 

[Loveall]

Anymore comments on what would be the downside of drying the EA? Like maybe not with a real drying agent, but mixing it with saturated NaCl solution and then separating layers again. Would not remove 100 % of water, but way more than the fridge step. What is then the downside of removing "too much water" from the EA prior to crystallization?

Cheeerss!

When completely dry the reaction doesn't go well. The TEK's
xtlas contain 1.5 molecules of water per molecule of mescaline, so water is a part of the process.

I think brine drying is a good idea. It may not work though, or it could leave just the right ammount of water for those struggling with the fridge decant, which requires some skill.

In the past, we have posted the % of water of EA in equilibrium with brine. Should be in the forum.

 

[Twilight Person]

Now I tried it with drying the ethyl acetate. Did this saturated nacl method, but outcome was exactly the same like before. This means I skipped the fridge water decant directly and put both the EA and the salt water into a sealed jar and shaked that stuff pretty strong. Then deparated it as much as possible, without spilling any salt water into the EA. I read it would not take 100 % of water, but most of it. So should be still keeping soooome water inside, but definetly less to make that slime at the bottom, instead of crystals.

Added the citric acid and it clouded nicely - which it also did the 2x failed cacti before

And now after already 1 day I just see slime again After day 3 just decanted everything. So apparently the water content did not play a big role here and I am simply doomed?

I told I tried to recover the mesc from that slime the last 2x times and just lost everything. So only explanation I would have in mind is that my cacti have no mesc inside? But at least one of them is from a smart shop bought in holland. So that really can't be ...

I now wanted to find out what this slime could be. I threw citric acid into wet EA and dry EA to see if it will also form a slime at the bottom. If not then my slime could be still a sign of mesc, which just forms a watery mess with that water (wherever it is from). If the citric acid would also form a slime at the bottom, then it would still be possible that all my cacti had no mesc ... because then this slime could also be just mostly citric acid. And now after 3 days the result is:

dry EA = nothing dissolved
wet EA = everything dissolved, no slime

So I guess this slime is still mostly mesc citrate, because citric acid would not form this layer? But then I have no idea why I lose it when I try to recover, maybe my chemistry is just not very refined.

Only hope I have now is using toluene from the beginning and throw inside benzoic acid, as currently there was a discussion again that it worked too. Should be independent of water content I guess. If that fails too, then I just have cacti with no mesc I guess. But feeling too scared to potentially waste a #4 of these precious plants

Anyways here is a picture of this slime again from 3rd cacti attached:

 

[Quetzal7]

Now I tried it with drying the ethyl acetate. Did this saturated nacl method, but outcome was exactly the same like before. This means I skipped the fridge water decant directly and put both the EA and the salt water into a sealed jar and shaked that stuff pretty strong. Then deparated it as much as possible, without spilling any salt water into the EA. I read it would not take 100 % of water, but most of it. So should be still keeping soooome water inside, but definetly less to make that slime at the bottom, instead of crystals.

Added the citric acid and it clouded nicely - which it also did the 2x failed cacti before

And now after already 1 day I just see slime again After day 3 just decanted everything. So apparently the water content did not play a big role here and I am simply doomed?

I told I tried to recover the mesc from that slime the last 2x times and just lost everything. So only explanation I would have in mind is that my cacti have no mesc inside? But at least one of them is from a smart shop bought in holland. So that really can't be ...

I now wanted to find out what this slime could be. I threw citric acid into wet EA and dry EA to see if it will also form a slime at the bottom. If not then my slime could be still a sign of mesc, which just forms a watery mess with that water (wherever it is from). If the citric acid would also form a slime at the bottom, then it would still be possible that all my cacti had no mesc ... because then this slime could also be just mostly citric acid. And now after 3 days the result is:

dry EA = nothing dissolved
wet EA = everything dissolved, no slime

So I guess this slime is still mostly mesc citrate, because citric acid would not form this layer? But then I have no idea why I lose it when I try to recover, maybe my chemistry is just not very refined.

Only hope I have now is using toluene from the beginning and throw inside benzoic acid, as currently there was a discussion again that it worked too. Should be independent of water content I guess. If that fails too, then I just have cacti with no mesc I guess. But feeling too scared to potentially waste a #4 of these precious plants

Anyways here is a picture of this slime again from 3rd cacti attached:

As i had the same problem, not managing to recover crystals, so i tried backsalting with vinegar instead of CA precipitation

I tried 2 different ways :
I blended fresh cactus and dried the soup in the sun
I blended fresh cactus, added lime, and dried that in the sun

Then reblended it in a mill
(the reason : it's super easy to blend fresh cactus, and it dried in 3 days in the sun ; i found it hard to blend dry cactus properly, or at least time consuming)

Here are the results (side to side experiment ,using the same ratio of lime, solvent, vinegar etc ; only thing that change is the drying condition and the type of cactus)

Dried old Scopulicola yield 1.8% black gooey liquid
Dried with Lime old Scopulicola : 0.383% solid dark redish paste
Dried 4-5 years sold bridgesii/peruvianus : 0.43% blakc gooey liquid
Dried with lime bridge/peruv : 0.21% solid reddish paste

Why does adding the lime as i'm drying the cactus, rather than just before extracting, changed completly the end results? i have no clue...

 

[Twilight Person]

Why does adding the lime as i'm drying the cactus, rather than just before extracting, changed completly the end results? i have no clue...

Could imagine this:

Although not having a watery paste the calcium hydroxide may still freebase huge chunks of mesc and then this is dried in the sun AKA high UV radiation on the freebase alkaloid. As far as I know all alkaloids are easily damaged by sun, even way more in their freebase form.

Maybe that is the reason?




And regarding crystallization I am now quite sure that the slime is still just pure mesc citrate. Still I have no clue why it does not form crystals, neither with fridge decant nor with that nacl water trick.

Now it starts slowly solidifying after I let it sit ventilated for 1+ week. Probably all the residual water / ethyl acetate gone and now starting to form crystals, although not really beautiful.

Still (if that is really mesc citrate) it does not help me much, because it will be a very thin layer on a really huge surface. Cannot scrape that up. I would probably need to dissovle it and then precipitate again.

What solvents could I use to recover that mesc here? Are there any solvents for dmt salts like fumarates which I could use here too maybe?

 

[shroombee]

Still (if that is really mesc citrate) it does not help me much, because it will be a very thin layer on a really huge surface. Cannot scrape that up. I would probably need to dissovle it and then precipitate again.

Could you use an eyedropper to add small amounts of water and slowly scrape into a pile? Then let the water evaporate.

 

[Twilight Person]

So now maybe I am just not really good at this, but my constant fails made me needing to practice what I can do if a slime forms instead of crystals. And now I have some information which may be useful for others, in case they encounter the same problem!!

Situation:
After doing the drying step of putting ethyl acetate into fridge, then you decant and the ethyl acetate should be water free. Then you dropped inside your excess citric acid, but already after 1 night you just get a slime at the bottom, which does not change during the next 3 days.

What you could do:
Do an extraction on this by dissolving in water, basifying, extracting back with organic solvent, add acid to create crystals.

DONT DO THIS! You will loose quite a lot of your goodies. This step seems ineffective. mesc (even freebase) seems to have a quite reasonable solubility in water, even more in basic environment (I saw clouds disappear when I went from pH 9 -> pH 12). I guess in the CIELO TEK it makes no problem, because you use an absolut minimum of water with many ethyl acetate pulls.

The good news is: It seems if you followed all the steps carefully with fridge-decanting water, then this slime at the bottom will be also water free. It just did not crystallize.

Instead of doing a real A/B you have 3 options:

#1
just wait and it will solidify on its own. Dont put it into fridge/freezer, this way it will solidify slower and therefore get harder probably. Still not the easiest stuff to handle, but it will get hard and you can weigh / handle it.
Pictures attached = 1-3

#2
do a "mini dry CIELO"
dissolve your slime in the absolute minimum amount of water
now throw on top like 3 g calcium hydroxide per 100 g powder (because apparently you cannot really weigh your slime mass). Then dry it 100 %. Maybe just leave it in a well ventilated (dark) area or put it into oven at 50 °C with ventilation on. Or put it into drying chamber with drying agent.
(caution: CaOH2 will get hot if you have big amounts thrown into water. If you have much material, better cool your vessel with a cold water bath, to avoid heating up mesc in its freebase form, which might damage it, in contrast to the salt form)

Then extract from this with your organic solvent of choice. I think if you just want to go for crystals and dont want to risk anything and not use dangerous acids, go with toluene and throw FASA on top. It seems to work I think? I dont have a chance to verify product, but it looks like a real salt and not just fumaric acid precipitated again.
This way you will recover close to 100 % of your mesc, while with a liquid-liquid extraction I always lost like a lot of it.

#3 (by far the easiest and best)
just do a ethanol or IPA re-x
heat the slime in boiling alcohol (probably both ethanol / IPA work the same way)
let it cool down to room temperature, then put it into fridge and then into freezer (as a sequence to create the biggest crystals).
If you dont use too much alcohol, then you can easily recover 80-90 % of your slime. You can alternatively evaporate off the last alcohol which you decanted after fridge in a second jar to get the last 10-20 %.
This will form nice white crystals and is probably the easiest method.
Pictures attached = 4

Now I dont know how many people might struggle with the same problem, I guess its a minority, but in case you run into the same situation you might use this. At least I am happy to get those insights, that's what I used my slime from 3rd extraction for after throwing away slime from 2nd and 1st haha! So dont have enough mesc to test it myself now, but I guess it was worth to get more insights for a potential extraction no.4.

Cheers

 

[Ruffles]

Did a CIXLO approach on 50 g dry T. bridgesii. In summary: Powder mixed into 100-120 ml sodium carbonate saturated water to make a paste (which eventually turned into a sticky goo - not the `sandy` consistency - the congealing part happened way too fast - high pH due to sodium carbonate?). Into paste, xylene was dropped and mixed with spoon as best as possible, no emulsion happened, paste absorbed some xylene into air pockets, xylene was recovered mainly by squeezing the xylene-paste-goo and then more xylene into it (200 ml total).

Squeezed out xylene was totally water-free and solid residues-free. Did lose about 50 ml of Xylene to the hungry green blobby goo paste, quite unfortunate. Don`t know how to recover it, will try adding lots of water to goo to see if it dissolves somewhat. Seems hopeless. Had a yellow tint to it. Of this, several 1 mL aliquots were taken into tubes for xyzASA attempts:

- FASA : Clouding instantly, powdery white precipitation dropped very fast, which has a tendency to clump. Xylene turned transparent after all precipitation dropped (strange, why ???)!!! Looks pretty good. UPDATE: Precipitates might require some centrifugation for full recovery.

- CASA : Instant clouding, gooey orange precipitation as droplets dropped really fast. Xylene remained yellow. Looks more like a HIELO than a CIELO. Will leave it in there for a while to see if it crystallizes. UPDATE: within bottom orange precipitate goo forms clumpy white crystals.

- MASA (DL-malic acid saturated acetone) : Instant clouding, white-orangey fluffy precipitates dropped almost instantly. Xylene remained yellow. This looks pretty good but not sure the magic really dropped out, could be malic acid dropping out, dunno. Have to wait till everything is over to do marquis. If it works then it beats FASA and CASA by a long long shot. UPDATE: Amazing needle white crystals are popping in walls of tube!

UPDATE 2: Marquis went brown on all three of the above. Hooray for MASA on xylene! Fastest precipitation ever.

- NASA (Nicotinic acid saturated acetone) : Didn`t quite look like it dissolved in acetone at all. No clouding in xylene.

- Concentrated sulfuric acid into 1 mL xylene, then mix : water droplet at bottom turned pitch black and xylene turned clear with a light blue tan.

- Considered doing Tannic acid ASA but this is a fixative that I do not want to mess with.



Thanks to all in this thread for sharing experiences!

 

[Twilight Person]

I think FASA on xylene / toluene is not very nice ... it is so (let's say) chemically repellent to fumaric acid, that crystal formation is so fast that it will never form big crystals. Impossible to get that pulver isolated without using a filter paper, and then it might absorb into the filter paper and be hard to recover.

But in general while xylene / toluene is not healthy and therefore not desired in contrast to ethyl acetate it gives a bigger spectrum of salting combinations, because I feel more stuff is crashing out from these 2.

 

[Twilight Person]

So now I found a really easy way to create the mesc benzoate, but it is simply from an already isolated batch of alkaloids ...

Take your mescaline freebase dissolved in limonene.

Take a second vial of 10 % that limonene volume only and dissolve like 1/2 (measured towards the mescaline content) benzoic acid while heating this limonene, it will not dissolve at ambient temp. Then just pour the hot benzoic-acid-infused limonene into the mescaline limonene and voila.

Instant clouding and super long crystals. How to identify it as the salt and not benzoic acid: Benzoic acid does not dissolve in water while the salt does. And also by just calculating the sum of the mass you will see that you get X+Y=Z mass of your precipitates, so it cannot be just one of the 2 components anyways.

Also limonene is super to re-x mesc benzoate. Solubility at room temp is 0 but limonene can easily be heated to 100 °C + and then solubility goes quite high. It will form crazy long needles like benzoic acid itself after re-x in limonene. Picture is attached.



But of course this is only given if you already have your isolated mesc. So now I wanted to move on and try using a mix of CIELO/69ron limonene TEK. Simply used cacti powder + 1/4 ca(oh)2 + small pints of limonene. And this is where the madness starts. It will just create an emulsion of hell. Absolutely no separation possible. Could not move on ...

And here it would be great if other member could tell me what has gone wrong. I just got into cacti like 1 year ago so CIELO is already well established. But many people have performed 69ron limo TEK and it was also a standard procedure. So why did it not separate in my case?

Afterwards I just threw more ethyl acetate on top, to not waste the cacti powder. Proceeded with the regular CIELO and will throw some citric acid on top at the end, hoping not getting a goo for 4th time. But can you tell me if emulsion has been a common problem for 69ron limo TEK?

Now here pictures:

picture 1 mes benzoate from freebase mesc + benzoic acid

picture 2 cacti paste while extracting with limonene, 0 % separation, 100 % emulsion

 

[shroombee]

So now I found a really easy way to create the mesc benzoate, but it is simply from an already isolated batch of alkaloids ...

Take your mescaline freebase dissolved in limonene.

What mescaline salt did you start with, and what process did you use to get mescaline freebase into the limonene?

But of course this is only given if you already have your isolated mesc. So now I wanted to move on and try using a mix of CIELO/69ron limonene TEK. Simply used cacti powder + 1/4 ca(oh)2 + small pints of limonene. And this is where the madness starts. It will just create an emulsion of hell. Absolutely no separation possible. Could not move on ...

And here it would be great if other member could tell me what has gone wrong. I just got into cacti like 1 year ago so CIELO is already well established. But many people have performed 69ron limo TEK and it was also a standard procedure. So why did it not separate in my case?

The 69ron paste typically absorbs a lot of the limonene on the first pull. And sometimes it's inconsistent - some pastes absorb more than others. That may the case here. What ratios of powder, water, and limonene did you use?

 

[Twilight Person]

First I had mesc citrate from CIELO, it was a goo so I recrystallized in ethanol.
= mesc citrate

Then I took that and freebased it. Instead of doing liquid-liquid extraction (dissolve in water, add base) which I found seems like a wasteful process as freebase mesc is also soluble in water, I instead made it a dry version. Mesc citrate mixed with a little water + ca(oh)2 and then I dried it to powder.
= mesc freebase + calcium citrate/hydroxide

Then pulled from that with limonene to only take up the mesc freebase. Dropped some benzoic acid dissolved in also limonene inside and nice crystals formed.
= mesc benzoate precipitation

The 69ron paste typically absorbs a lot of the limonene on the first pull. And sometimes it's inconsistent - some pastes absorb more than others. That may the case here. What ratios of powder, water, and limonene did you use?

Ratio was exactly the same like 69ron, which is actually the same like for CIELO. I wrote here:

Simply used cacti powder + 1/4 ca(oh)2 + small pints of limonene

Also it was ~300 ml water for 100 g cacti powder. Limonene shots 50 ml per pull.

Good to know you say for some other people it also just absorbs. But I have to say it did not even look as if there could be any separation ever. Which seems strange to me as this process was also used all over the place if I read back in time.

 

[shroombee]

First I had mesc citrate from CIELO, it was a goo so I recrystallized in ethanol.
= mesc citrate

What percentage ethanol did you use? And I assume you needed to boil the ethanol as you mentioned in the other thread?

Ratio was exactly the same like 69ron, which is actually the same like for CIELO. I wrote here:

Simply used cacti powder + 1/4 ca(oh)2 + small pints of limonene

Also it was ~300 ml water for 100 g cacti powder. Limonene shots 50 ml per pull.

Good to know you say for some other people it also just absorbs. But I have to say it did not even look as if there could be any separation ever. Which seems strange to me as this process was also used all over the place if I read back in time.

The 69ron TEK calls for 300 ml limonene for 100 g powder.

It's been a while and I don't have my notes handy, but I believe sometimes 150 ml of limonene is absorbed on the first pull. So if you only added 50 ml limonene it's likely to all be absorbed. It's not possible to squeeze out the absorbed limonene, no matter how hard you try.

 

[Twilight Person]

Yes boil it at 80 °C with the minimum amount and and then it goes straight to the freezer! It was pure Ethanol or let it be 98+ % of course.

Maybe 98+ % IPA has the same effect?

About using more Limonene, yes after the first did not separate I of course threw more on it :/ But quickly I realized upon adding more and more it will not do for the better. Then before I got a 10x volume of sludge emulsion I switched to ethyl acetate and pulled from that remaining stuff.


Fun fact is I then proceeded as normal and again just got goo. Sadly I am really doomed with CIELO too Seems like a systematic error, but it is ca(oh)2 and perfectly dried / ground cactus powder. Afterwards pure ethyl acetate and even the citric acid monohydrate. But now I accepted to just get goo and just perform a re-x afterwards. Will not make the same mistake again like the first tries and pour that goo off, which I believed to be still excess water :?