• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

TEK Ethyl acetate approach [CIELO]

This topic contain a TEK
Migrated topic.
Hi.

I have approximately 1kg of 3x lysed green pulp in the freezer. I was studying CIELO TEK, but it seems that it doesn't work for me...

I thought about taking the green pulp, boiling it with water for 2 hours in a pressure cooker, filtering it, basifying it with NaOH and extracting the liquid-liquid with EA.

and then continuing with CIELO.

Could anyone comment?
That sounds like problems. If you can, spread the pulp out thinly on baking sheets or similar and dry it. Airflow is better than heat, and this may take numerous batches over several days.

Once the pulp is cracker dry it can be powdered and stored - of course, you can powder the first batch while the second batch is drying, and the more trays that you can use, the sooner this gets done. And once you have sufficient powder you can then proceed with a standard CIELO.

Drying has been found to alter the cactus mucilage in such a way that it becomes much easier to work with as a lime paste. Treating fresh pulp with lime (for example) produces difficulties, partly on account of excess water and largely because of its terrible sliminess. This is why cactus extraction typically involves prolonged boiling ((n)), or drying of the cactus material.
 
You cannot use lye with the EtOAc as it will break down the solvent into alcohol. You should get calcium hydroxide for Cielo. If you want to use NaOH you should use xylene. I believe limonene also worked with lye.

If you want to do cielo you could cook down the tea as much as possible without it become too thick then adding calcium hydroxide. You will need to use the freezer method to remove excess water from the ethyl acetate after doing liquid-liquid extraction. It'll work just slightly extra work

EDIT: Also careful using the Pressure cooker with cacti. I use it each time but FIRST COOK until there is no more foaming/snot. If you don't precook for around 30 minutes it may clog the valves on the pressure cooker leading to possible excess pressure and safety issue.
 
Last edited:
That sounds like problems. If you can, spread the pulp out thinly on baking sheets or similar and dry it. Airflow is better than heat, and this may take numerous batches over several days.

Once the pulp is cracker dry it can be powdered and stored - of course, you can powder the first batch while the second batch is drying, and the more trays that you can use, the sooner this gets done. And once you have sufficient powder you can then proceed with a standard CIELO.

Drying has been found to alter the cactus mucilage in such a way that it becomes much easier to work with as a lime paste. Treating fresh pulp with lime (for example) produces difficulties, partly on account of excess water and largely because of its terrible sliminess. This is why cactus extraction typically involves prolonged boiling ((n)), or drying of the cactus material.
It seems like a lot of work. I'll try another tek on this batch.
 
You cannot use lye with the EtOAc as it will break down the solvent into alcohol. You should get calcium hydroxide for Cielo. If you want to use NaOH you should use xylene. I believe limonene also worked with lye.

If you want to do cielo you could cook down the tea as much as possible without it become too thick then adding calcium hydroxide. You will need to use the freezer method to remove excess water from the ethyl acetate after doing liquid-liquid extraction. It'll work just slightly extra work

EDIT: Also careful using the Pressure cooker with cacti. I use it each time but FIRST COOK until there is no more foaming/snot. If you don't precook for around 30 minutes it may clog the valves on the pressure cooker leading to possible excess pressure and safety issue.
I didn't know about this incompatibility of Ea with NaOH. But would it be possible to make an A/B with CaOH and EA?

or can I basify with NaOH and pull with xylene or limonene (I prefer d-limo) and then salt with FASIPA?
 
Last edited:
It seems like a lot of work. I'll try another tek on this batch.
You're in the perfect position to split your pulp into two batches and run them through a different method each. Then you might find out if the dehydration route really is more work. It's pretty easy once you've got to the stage of cactus powder.

But how pulpy is your pulp? If it's actually chunks, for example, that could make things easier. Strips would be even better.

The completely 'out there' (not to mention wholly untested and potentially dangerous*) option might be to mix the pulp with calcium oxide, which would reduce the water content while forming calcium hydroxide in situ. CaO reacts with about a third of its weight of water, so 75g of it would be the equivalent of adding nearly 100g lime, and would use up a little less than 25g water.
[*only from the heat of hydration, which can be controlled via the rate of addition.]

Your A/B route would involve lengthy boiling and straining of the cactus material - or have you envisaged the acidic step a different way? It may be wise to weigh up just how much work each option might be, since IME the boiling of cactus can become quite tedious, unless perhaps you're sat around a ceremonial fire preparing a brew for direct consumption.

would it be possible to make an A/B with CaOH and EA?
This would appear to involve the aforementioned boiling, followed by some not inconsiderable evaporating-down of the resulting brew(s), but once you get up to or beyond the stage of syrupy resin it seems possible to mix in lime and attempt the EA pulls.

can I basify with NaOH and pull with xylene or limonene (I prefer lime) and then salt with FASIPA?
From what I've heard, this could lead to emulsion problems during the basic pulls, but it still resembles a viable reaction scheme on the face of it. Is there a reason for your choice of FASI? Do you have access to benzoic acid?
 
You're in the perfect position to split your pulp into two batches and run them through a different method each. Then you might find out if the dehydration route really is more work. It's pretty easy once you've got to the stage of cactus powder.
It's something to consider... I might try drying it on baking sheets in the fridge.

can I basify with NaOH and pull with xylene or limonene (I prefer lime) and then salt with FASIPA?
From what I've heard, this could lead to emulsion problems during the basic pulls, but it still resembles a viable reaction scheme on the face of it. Is there a reason for your choice of FASI? Do you have access to benzoic acid?
Benzoic acid is controlled here in my country...
Fumaric acid and IPA are easy to get.
 
It's something to consider... I might try drying it on baking sheets in the fridge.


Benzoic acid is controlled here in my country...
Fumaric acid and IPA are easy to get.


Benzoic acid can be easily made from sodium benzoate. Simply dissolve sodium benzoate in hot water and add HCl and benzoic acid will crash out immediately. You can calculate the amount of HCl needed for this reaction, but I'm too lazy to do that, so I just eyeball it, then filter out the left over water, add some more HCl to it and see if anything crashes out. The benzoic acid can further be purified by recrystallization from boiling water. Simply dissolve it in boiling water, let it rest and cool down over night, pour out the water, collect and wash the BA crystals with small amounts of cold water and dry them.
 

Benzoic acid can be easily made from sodium benzoate. Simply dissolve sodium benzoate in hot water and add HCl and benzoic acid will crash out immediately. You can calculate the amount of HCl needed for this reaction, but I'm too lazy to do that, so I just eyeball it, then filter out the left over water, add some more HCl to it and see if anything crashes out. The benzoic acid can further be purified by recrystallization from boiling water. Simply dissolve it in boiling water, let it rest and cool down over night, pour out the water, collect and wash the BA crystals with small amounts of cold water and dry them.
Thanks for the tips. I'll study this tek.
 
Look into CITLO Mescaline benzoate: Cactus/Lime/Toluene/Benzoic acid

Xylene can also be used
Thanks for that link. I think I'll attempt this as someone mentioned they used lye and you mentioned xylene can be used :) If this works and I can skip the evaporation of the hcl water it's a win for me. Also I love the dmt benzoate and how I can clean it perfectly with 99+% isopropanol. Reading the thread the solubility seems mixed. I'll attempt myself.

I tired using 99% iso as the main solvent but due to poor penetration and breakdown of the plant material and requiring completely dry solvent I had poor results. BASI is interesting but not practical atleast how I've done it so far.

Cactus/Lye/Xylene/Benzoic acid will be awesome for me :) Just not sure if I need to 'dry' the xylene or not for it to precipitate.

EDIT: someone mentioned adding more acid resulted in more powder... I suspect it is the same think as added excess hcl acid leading to impurities/other alkaloids since ph goes down to 2.5? Regardless I'll update when I get around to testing myself.
 
Another practical option is to precipitate alkaloid salt from toluene/xylene with xASy method.
(where x = citric/tartaric/fumaric and y = ipa/ethanol/acetone)
I prefer and use tartaric, as mescaline tartrate is great for re-x.
 
Is BA interchangeable for EA in cielo tek transform?
Almost - it may be better to add the citric dissolved in acetone, though, or the BA seems to need active wetting with a bit of distilled water. A bit hazy recalling exactly, but dissolving the citric in wetted BA prior to adding to the cactus BA extract was also an option explored.
 
"Not yet!" 😁
In that respect it would be wise to dig around a bit for some solubility data for other (solid, organic) acids in BA.
I remember doing tests on BA unsure if I posted data on it. Better do some digging.


Edit:
"Butyl Acetate although holds benzoic acid well, it also holds DMT benzoate as well so is not a good combo. BA doesn't hold other acids well unless wet. Tested malic, tartaric, citric, lactic, fumaric.
Did not test hcl or phosphoric" don't take my kitchen chemistry as reliable but those may need some confirmations. Wonder if mescaline benzoate would precipitate?
 
Last edited:
Wonder if mescaline benzoate would precipitate?
That, essentially, is the question that has been hanging at the back of my mind too, although the solubility of DMT benzoate makes this seem less promising. Another possible one to try is succinic acid. Beyond that, the organic acids start getting relatively obscure, other than oxalic acid, which is probably unsuitable, and malonic acid, which is a controlled precursor in many places. Adipic acid crops up from time to time and would conceivably be worth a try too.
 
Back
Top Bottom