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TEK Ethyl acetate approach [CIELO]

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Twilight Person said:
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?
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Could you try IPA? You might have developed a reliable method for recovering goo that we could add to the TEK. IPA is easier to obtain (and cheaper) than 190 proof ethanol.

Fun fact is I then proceeded as normal and again just got goo. Sadly I am really doomed with CIELO too :cry: 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 :?
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Try adding excess ethyl acetate to the pulls before adding citric acid. I was always successful getting xtals and the one outlier in my technique is using excess ethyl acetate. It's a theory that hasn't been tested yet (AFAIK).
 
Twilight Person said:
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 :cry: 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 :?
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What is the temperature of the EA when you salt and the temperature of your fridge?
 
I have checked IPA with some small residues which I still have and seems to work the same way. Allthough not sure about how efficient crystallization was, dont have much and my scale might become inaccurate.

About excess ethyl acetate: I have followed the TEK always close and lastly I just had a super tiny amount of cacti powder, still used a big load of solvent. I think I had like 300 ml at the end from just 15 g cacti. Still same goo. It's so strange I have used 4 different cacti now all with the same result.

About the temperature: I set the fridge even a little colder just to be sure. Thermometer showed 5° instead of 8°. And then I always place it out of fridge like the TEK is telling, before start salting.

It's pretty annoying to not succeed but now I dont care anymore because I turned at least that goo into crystals, that I did not throw away :roll: :roll: :roll: I did my best trying things with toluene and limonene, but it was not reliable so my personal way might be just going CIELO and even if I get goo every single time just use that ethanol. :thumb_up:
 
Twilight Person said:
I have checked IPA with some small residues which I still have and seems to work the same way. Allthough not sure about how efficient crystallization was, dont have much and my scale might become inaccurate.
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If we can confirm IPA works as well as ethanol, and others can repeat the process, at least we'll have a goo recovery technique we can add to the TEK. What does the final product look? Easy-to-handle xtals?

About excess ethyl acetate: I have followed the TEK always close and lastly I just had a super tiny amount of cacti powder, still used a big load of solvent. I think I had like 300 ml at the end from just 15 g cacti. Still same goo. It's so strange I have used 4 different cacti now all with the same result.
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Okay, that probably puts the "excess EA" theory to bed.

It's pretty annoying to not succeed but now I dont care anymore because I turned at least that goo into crystals, that I did not throw away :roll: :roll: :roll: I did my best trying things with toluene and limonene, but it was not reliable so my personal way might be just going CIELO and even if I get goo every single time just use that ethanol. :thumb_up:
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The benzoic acid in limonene was not reliable?
 
Can confirm the Ethanol re-x worked for me, I just ran my first CIELO extraction on 100g bridgessi and got a crystalline brown oil after salting, after separating EA and leaving the goo to dry, I heated 30ml of 95% Ethanol to the boil and added it to the goo, I force stired the brown oil into the Ethanol, immediate separation of the goo and mescaline citrate occurred, with the goo dissolving into the Ethanol, I decanted that through a coffee filter to collect the white powdery xtals and put the Ethanol goo in the Freezer for 24h, some more crystals formed during that time which I filtered and dried and then evaped the remaining ethanol to yield small residue of brown oil which I might just add to the next extraction incase of any remaining mesc inside.

Overall my yield was pretty low 0.7% mesc (700mg), but I did really mess up the consistency to begin with, the 250ml water and lime paste was way too much water (oatmeal soup), so I had to add alot of extra lime to reach mash potato consistency and could have done a few more EA pulls but I ran out.. next extraction I know will be better and goo is no worries because ethanol re-x is so easy to do and works well.

I also have a feeling over salting bridgessi extracts will cause brown oil/goo to drop out due to bridgessi's large alkaloid profile so will try to use minimum amount of citric acid needed for xtalisation.
 

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I was surprised also, maybe I didn't wait long enough for the paste to congeal but I couldn't see it thickening up that much..I used the whole bridgessi plant except the core (one of then was slightly rotten but was dried to a crispy cracker), I dried it over a week infront of a woodfire chopped up in small chips, I then powderised the chips in a vitamix blender, it was fine enough to look like vapour..I will try again in the next few days and see if I get the same result
 
Regarding the creation of benzoate salts and the discussion of drawing benzoic acid into the product, here is some data:

The solubility of benzoic acid in those solvents is as follows

Benzoic acid in Toluene (20 °C):
70 mg / 1 ml
0,7 g / 10 ml

Benzoic acid in Limonene (20 °C):
47 mg / 1 ml
0,5 g / 10 ml

This means as long as you would have an extraction from 100 g cacti and the expected solvent (now Toluene or Limonene instead of EA) at the end would be 800 (200 + 5x125) g (which should be 1000 ml) and you will add also 5 g (excess) benzoic acid (probably not needed because you will anyways create the mono-valente salt) the 5 g will definetly stay in solution. So in a regular extraction it would not even be possible to get benzoic acid into the final product, even in limonene solubility will be high enough.

Now I retrieved some Meskalin Citrate to make some experiments with it! Solubility was one of the first, but also all kind of other stuff done so expect the final chapter to the Chemical Guide coming soon :love: As it seems solubility is quite high of Meskalin Benzoate in Toluene, because of this it would be mandatory to reduce the volume ... and reducing volume of some organic solvent for a smooth TEK is not really classy :oops: :oops: Actually this is really weird, because solubility of DMT Benzoate is really low in Toluene. And moving from DMT to Mescaline not only the logP already tells that it is much more polar: Simply judging by eye you migrate from -NMe2 -> -NH2 and also add 3x Ether groups. This should also make the overall salt Mescaline Benzoate way more polar than DMT Benzoate and thus make it precipitate much easier even in Toluene ... :? In contrast stuff that would increase solubility in Toluene would be more double bonds or thiols / halogens attached to the ring. But that is not the case.

Limonene on the other hand has a solubility of nearly 0 for the Meskalin Benzoate. But then it would be interesting if people can confirm that separation from paste and limonene is indeed as easy as written in 69rons TEK ...
It could have the beauty of being inaffected by water content, so crystallization might be more fool proof. Still solubility might be better inside of the Limonene retrieved from an extraction than from Limonene that only carries the Alkaloid salt. Reason is if retrieved from a plant extract it will still have more oils and fats from the plant (which are left behind by salting) that could act like a coalescing agent and actually increase the salt solubility. So based on my pretty great crystallizations of Mes.-Benzoate in Limonene it is not safe to say if it would work the same in the Limonene from a plant extraction.



Lastly on the IPA/EtOH-rex:

Solubility seems pretty fitting for an easy process. Will post data soon with all the other diagrams. But it is reduced to < 20% in the Freezer compared to boiling, so it is not a wasteful process. But even more it seems as this goo (if you will get any) from CIELO is still mostly pure Meskalin Citrate.

I believe the problem here is not a wrong fridge decanting. Because I feel that this goo is free of water. It simply did not crystallize properly. Because of that it also does not contain any amount of unreacted citric acid, instead it is left behind in the EA that you decanted. That has the great benefit of simply evaporating all the IPA/EtOH instead of doing the rex in the Freezer. This way you also get crystals, but you will not loose any Alkaloids which did not precipitate. And even if your goo WOULD contain some water, it will co-evaporate with the alcohol, as it forms azeotropes with water and therefore also pull it out while evaporating down.


So regarding Mescaline Benzoate it would be interesting to receive it as an alternate salt option, but it seems to be somehow limited by not precipitating from 500+ ml Toluene and Limonene might not separate as nice as EA. Still it would be an interesting option, as I think from all the possible alkaloid salt combos Benzoic Acid is giving the superior properties to the compound. I checked evaporation on M-Citrate / M-Fumarate / M-Benzoate and M-Benzoate evaporates neatly like Freebase DMT even, same temperature and no combustion. That is now an interesting thing to test!

But apart from this property it seems as boiling your goo in IPA and evaporating it is just fine to solve all other potential problems.
 
Fruit is life said:
I was surprised also, maybe I didn't wait long enough for the paste to congeal but I couldn't see it thickening up that much..I used the whole bridgessi plant except the core (one of then was slightly rotten but was dried to a crispy cracker), I dried it over a week infront of a woodfire chopped up in small chips, I then powderised the chips in a vitamix blender, it was fine enough to look like vapour..I will try again in the next few days and see if I get the same result
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I'm not familiar with woodfire drying, perhaps that makes a difference.

Earlier you mentioned you used minimal amount of citric acid, that is not reccomended. You want extra to citric to make conditions acidic during xtalization and form momo-mescaline citrate. With less citric, di or tri mescaline citrate can form in the form of goo from EA.
 
Fruit is life said:
Can confirm the Ethanol re-x worked for me, I just ran my first CIELO extraction on 100g bridgessi and got a crystalline brown oil after salting, after separating EA and leaving the goo to dry, I heated 30ml of 95% Ethanol to the boil and added it to the goo, I force stired the brown oil into the Ethanol, immediate separation of the goo and mescaline citrate occurred, with the goo dissolving into the Ethanol, I decanted that through a coffee filter to collect the white powdery xtals and put the Ethanol goo in the Freezer for 24h, some more crystals formed during that time which I filtered and dried and then evaped the remaining ethanol to yield small residue of brown oil which I might just add to the next extraction incase of any remaining mesc inside.

Overall my yield was pretty low 0.7% mesc (700mg), but I did really mess up the consistency to begin with, the 250ml water and lime paste was way too much water (oatmeal soup), so I had to add alot of extra lime to reach mash potato consistency and could have done a few more EA pulls but I ran out.. next extraction I know will be better and goo is no worries because ethanol re-x is so easy to do and works well.

I also have a feeling over salting bridgessi extracts will cause brown oil/goo to drop out due to bridgessi's large alkaloid profile so will try to use minimum amount of citric acid needed for xtalisation.
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Thanks for sharing, i was just asking myself if i can crystalize mesc critrate ; i guess IPA should work the same (i can get 99% here)

what's your favorite way of recovering the goo out of the CIELO? just pour out the EA , add a bit water and evaporate ?
 
I retrieved some other goo to test around and tried to convert it to Mescaline Benzoate, yet no precipitation and thus only Benzoic Acid after evaporation ... means in this other goo I had no alkaloids inside :((

The weight of the goo / Ca(OH)2 mix stayed exactly the same even after pulling with Toluene and Aceton. So that seems like no Alkaloid was extractable.

But then I got a strong Freebase Smell like after adding NaOH to a DMT extraction. So that MUST hint about it containing Alkaloids?

Sadly I dont have any way to analyze it currently (and anyways used up the last bit of what I was given). So still no idea if it truly contained Mescaline or not ... it smelled like it, but nothing was carried over after Freebasing (which definetly worked).




But in order to check if that goo might be just partially or complete Citric-Acid-Water-Mix instead:

I placed some goo in water before, dissolved completely, checked pH. It was not acidic. So must be a salt instead.

Next up check if it is even possible, that Citric Acid will "leave the EA" and separate as some goo with some of the water from wet EA (from mixing with water).

1. So mixed some 100% EA with some water, separated, (did not even fridge dry it,) then added citric acid.

2. As a control also did the same with 100 % EA.

Interestingly after 48 h in 1. everything was dissolved. No goo even with the "big load" of water without fridge decant.

But in 2. no Citric Acid was dissolved. It just stayed as crystals at the bottom.

So I feel that even with a lot of water, Citric Acid seems not to separate and form a goo (with that water) at the bottom. Instead just stays dissolved - at least for the "pure mix", about the cacti-derived no idea.

But because of that I think it is pretty unlikely that this goo would be just (or mostly) Citric Acid, that would require separation from any potential Mescaline Citrat.

Still then no idea why I could not extract anything from that last goo that I had ...
 
While doing my trials during the last time I was just curious experimenting with the mixing step. I guess this will be the one that is responsible how well the extraction from thne paste is going. The more mixing the better. So insted of using a spoon I was using a regular kitchen mixer. With my one d-limo trial it caused an emulsion of hell instantly. That was when I could not separate anything anymore, even with more d-limo.

But with ethyl acetate it works still brilliant, not forming any emulsion, no matter how hard you mix. Attached is a picture, maybe also try it. This can only make the mixing step more effective. Interestingly even in a big bowl there was absolutely no spilling of liquid.

Now as you cannot reach with a kitchen mixer into a french press, I was also doing the decant step in a different way. As long as the paste is not slimy, you can simply put it onto a kitchen sieve, wait for all the EA to drop off into your collector pot and then put it back into the bowl for 'kitchen mixing'. Very easy and also fast.

Cheers
 

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I used an emulsion blender that fit perfectly into my french press and it worked well. About half way through my 2nd mason jar it became too slimy to use the blender though.

The cactus I had was bunk. The citric acid monohydrate I added didn't trigger the growth of any xtals and instead left me with a goo at the bottom, which I collected with hot water then evapped but it was still just a goo, I collected it, dunno what dose it is and I'm scared to ingest it. Could have been the cactus, or maybe because I ground the monohydrate crystals into a fine powder. Idk.

I have a new batch of cactus now, Trial 2 starting soon.
 
If endlessness endorses this one has to give this a try. Recently acquired some cacti powder so one can finally give this a go! Eager to see the results. :D

Cheers Loveall.
 
Loveall said:
Thank you! Hope you enjoy the process 😊
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Too far back to dig up the post from 6 months ago but I believe I had followed the steps incorrectly because I used 10g of citric acid monohydrate instead of the recommended 5, (And you rightfully called me out on that) and I also used my coffee grinder to powder the CA as I thought maybe it would dissolve faster but it ended up just clumping on the bottom.

For my second run I will use 5g and not powder.

I believe I also used 230mL of water when liming the cactus powder. I for one have a difficult time determining what "mashed potato" consistency is because I enjoy my mashed potatoes both thick AND super creamy. My viscosity tastes are wide ranging lol.

Perhaps anyone on here listening can post photos of their consistency while doing their extraction? I fear I should have gone with 250mL. The cactus I have is hard to grow in my region, and I really want to get this next extraction right as it's my last 100g.

It's funny, I've nearly perfected DMT extraction, so I find it embarrassing that I struggled with the CIELO which on paper is so simple and effective, and I thank you for that Loveall.
 
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