• 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.
Which botanics, with a view to recovering which substances? Some will work, some won't, and yet others will require variation of methods, likely to the point of not really being CIELO any more.
You should be able to get many/most alkaloids since most are basic in nature with some exceptions. The issue you may get is salting with citric acid as that alkaloid citrate may or may not be soluble in the ethyl acetate. Most papers do not even attempting salting they evaporate the solvent completely then research as freebase or salt here after solvent is recovered. You could also add an acid water to pull the now acidic alkaloid back to the water.
like transform mentioned at this point it isn’t really even Cielo anymore and just using ethyl acetate as the solvent.

Edit: I replied to the wrong post but still works. :)
 
Last edited:
Laying out the general principles of what we call CISLO (which has its own thread) we have: base treatment of plant material in paste form; solubilisation of freebase alkaloid in broadly water-immiscible NPS; salting of alkaloid with at least weakly NPS-soluble acid; formation of NPS-insoluble alkaloid salt ideally in crystalline form (DMT citrate forms an oil, just as an example of other possible outcomes).
Search: [threads] CISLO

A three-dimensional (at least) spreadsheet would be required for comparing combinations of alkaloid, NPS and acid. Sounds like fun 😁
 
My OTC EA option here in the EU has been acetone-free nail polish remover, although I've held back on the refining process after discovering a supply of butyl acetate. Butyl acetate [BuOAc]
(a.k.a. 'banana oil') picks up mescaline freebase quite well, but there are a few challenges because of the poor solubility of citric acid in comparison with using EA. This can be overcome by using a solution of citric acid in some other solvent, like acetone ("FASA)" or isopropanol ("FASI"). Acetone, in particular, is fairly easy to separate from BuOAc by distillation. IPA might require a fractionation column (e.g., Vigreux) for a quicker, cleaner separation (i.e. for re-use of the BuOAc).
why would one need to seperate them tho?

i also dont understand why the tek requiers only ea (probout of ignorance), hence would love an explanaion:))
i just assumed mek, , acetone basically the ketone family and their relative would work more or less close to each other

like why not get fumaric and use acetone which is super easily available to everyone would it be the same and youll get a stronger product too AND you will not need to worry about the water ratio for formation of xtals since there is not water molecule in mascaline fumarate unlike Mcitrate.....?🤔
 
Last edited:
You might want to read back through the thread. The point of this tek is that you can quickly extract high-purity mescaline in a few relatively straightforward steps.

Your proposal to do an extraction with fumaric and acetone is an option, but it's a different tek. It's like going onto a limonene DMT extraction thread and suggesting a freeze precipitation with naphtha. That's a fine route, but it's not what the thread is about.
 
Last edited:
why would one need to seperate them tho?
You need to do some basic reading comprehension:
Acetone, in particular, is fairly easy to separate from BuOAc by distillation. IPA might require a fractionation column (e.g., Vigreux) for a quicker, cleaner separation (i.e. for re-use of the BuOAc).
Context is everything here. Starting with, as @Memberberries points out, the title of the thread, followed by the particular tangent of the discussion at this point. Acetone is used as a better solvent for citric acid than butyl acetate, and can be separated easily on account of the relatively large difference in boiling point between the two components. (Azeotropes notwithstanding? Fortunately not - they even give zeotropic distillation, as does the BA/IPA mixture :) )

P.S. - substituting BuOAc for EA (EtOAc) seems like a reasonable adaptation remaining within the context of CIELO. The introduction of a second solvent does, admittedly, turn it into a CISLO-CASA hybrid.
 
The TEK has been updated based on experimental user feedback.

It now recommends less water (yet again) to make a wet crumb mix with the cactus powder/lime/water instead of a dough.

It is believed ideal wet crumbs should stick together when cupped and crumble when broken apart. This way loose parties will not be released (since the mix is wet enough) and goo is less likely to form instead of xtals (since the mix does not have too much water).
 
Thanks a lot for this! Some pics of said wet crumbs would be greatly helpful as visual aid. I am about to try this Tek for the first time. Much love from oneness.
 
So In that paper they explore citric acid and other green solvents to test extraction of alkaloids. They only have a peak half the size of traditional extractions using other solvents and reference of methanol hcl.

The ethyl acetate was used to “defat” the polar compounds in a citric water extract of the cactus. Then based with ammonia and pulled again with ethyl acetate for a pure extract. The way Cielo is structured you pull polar and freebased alkaloids. If you look at the hplc the citric water extract has a high early peak compared to methanol hcl control reference.

This half yield would fix discrepancies in yields of high citrate.
 

Attachments

  • acs.jnatprod.pdf
    2.3 MB · Views: 11
Posting this exchange about sediment in the solvent with Loveall from reddit here for searchability:

Me:
What's an acceptable amount of particulate in the solvent? I decanted the much cleaner jar, leaving behind sediment and some water drops, and let it rest again.

Today, I couldn't tell between particulate and soda glass imperfections. Swirled it, observing sparse particulate. Upon closer inspection, there is difficult to see particulate suspended in the solvent, but I'm unsure. It looks very clear, save for a few larger particles here and there visible by flashlight. Do I have to be very thorough in removing virtually all particles that I can see with a flashlight?


Loveall:
Up to you, the more you remove the better.

Just keep in mind that whatever you don't remove you may consume. Lime particles will become Calcium Citrate and cactus particles will just be cactus powder.

Use whatever your comfort level is. As far as the process goes, at this time the small amount of debris should not interfere with xtalization.

When you collect the xtlas, you may have another chance at separating impurities. The xtals should drop down faster than impurities so decanting carefully may help. After that use fresh EA to agitate the xtals into the solvent and send them through a filter for collection.


Original post for reference.
 
Idk if anyone talked about it already,
but i guess that in different climates/seasons unless your environment is all the way in a stable temprature always,

Shouldnt that effect the whole water ratios up until the saltings?
I dont mean of the dough of course but of the fridge rest or taking water in any other way..





*Btw did anyone have a bad experience with MgSO4? Its not recommended in the tek i was wondering why

*thought about freezing the EA and then adding water by weight
Seems foolproof, what do you guys think ?
 
Last edited:
Idk if anyone talked about it already,
but i guess that in different climates/seasons unless your environment is all the way in a stable temprature always,

Shouldnt that effect the whole water ratios up until the saltings?
I dont mean of the dough of course but of the fridge rest or taking water in any other way..





*Btw did anyone have a bad experience with MgSO4? Its not recommended in the tek i was wondering why

*thought about freezing the EA and then adding water by weight
Seems foolproof, what do you guys think ?
There are some that do this and have high success. The issue with chemical drying is excessive removal of water and possible small loss of yield if excess drying agent added. I did sodium sulfate drying in the past but I’ve always had issues with Cielo so my experience should be used.
 
So In that paper they explore citric acid and other green solvents to test extraction of alkaloids. They only have a peak half the size of traditional extractions using other solvents and reference of methanol hcl.

The ethyl acetate was used to “defat” the polar compounds in a citric water extract of the cactus. Then based with ammonia and pulled again with ethyl acetate for a pure extract. The way Cielo is structured you pull polar and freebased alkaloids. If you look at the hplc the citric water extract has a high early peak compared to methanol hcl control reference.

This half yield would fix discrepancies in yields of high citrate.
They are comparing vs. Chloroform not methanol.

Half the yield in the first pull of a LLE extraction does not imply anything for CIELO yields.
 
Idk if anyone talked about it already,
but i guess that in different climates/seasons unless your environment is all the way in a stable temprature always,

Shouldnt that effect the whole water ratios up until the saltings?
I dont mean of the dough of course but of the fridge rest or taking water in any other way..





*Btw did anyone have a bad experience with MgSO4? Its not recommended in the tek i was wondering why

*thought about freezing the EA and then adding water by weight
Seems foolproof, what do you guys think ?
Yes, environments can affect the process.

MgSO4 dries the extract too much. Freezing does too.

Yes, adding water back or being letting some ice melt while separating is successful for some people. This is not supported by the TEK.

Have you tried the wet crumbs? They should work
 
They are comparing vs. Chloroform not methanol.

Half the yield in the first pull of a LLE extraction does not imply anything for CIELO yields.
You did mention that with cielo you pull to exhaustion I guess. But the LLE is from an already concentrated extraction and I don't see how it would cause an issue... Do you know the solubility of freebase mescaline in EtOAc maybe it was saturated at that volume?

With cielo you pull other alkaloids and a 'defat' step doesn't only remove fat but also other alkaloids. With the paper not having the HPLC of the citric acid ethyl acetate extract hard to say directly. The Methanol fraction was defat and pulled with DCM and still had impurities.

The logic with the DCM citric acid fraction being very clean could be associated with it being less polar than ethyl acetate. I could be completely off base. I'll just wait for someone to test free the M citrate with HCL and then a cleanup to verify. Should be close to the theoretical conversion weight of the Mescaline freebase.
 
Loveall mentioned there was someone on the Nexus that did a freeing of the Mescaline citrate and conversion and got the hcl conversion with the expected weight.... If someone could find it and link here would be awesome. I've searched a few times and haven't found it.
 
Loveall mentioned there was someone on the Nexus that did a freeing of the Mescaline citrate and conversion and got the hcl conversion with the expected weight.... If someone could find it and link here would be awesome. I've searched a few times and haven't found it.
I'll have to guess it wasn't nny of these?

It seems difficult to get the right search terms, at least with the Nexus search function. Have you also tried an external search engine?
 
I'll have to guess it wasn't nny of these?

It seems difficult to get the right search terms, at least with the Nexus search function. Have you also tried an external search engine?
Someone had a pdf of this chat and it helped a lot

#380, #398, #404-410

Yea it seems trips did the conversion doing mini kash and was indeed high purity yielding expected amount of hcl salt.

I mean now I'm even doubting my 'non-mescaline' alkaloids since I did a re-crystallization today and I got some very dark crystals that didn't dissolve. And the iso99 that I evaporated looked like mescaline lol. I'll be doing the TLC on each separately. I'll re-x the dark crystals in water and see how it looks. I'm gonna try a different approach rather than using hcl with the xylene I'll use a citric acid water.

I'm thinking that different 'forms' of mescaline may be possible... when researching the 'SOMA' publications the dmt and 5-meo-dmt were found in different fractions including "water soluble base alkaloids". Perhaps the ethyl acetate with citric acid is able to precipitate all the mescaline forms either a property of the solvent or the citric acid.

I don’t quite understand quaternary alkaloids since it’s the same alkaloid but water soluble base alkaloids? Will be my next research to better understand
 
Last edited:


Write your reply...
Back
Top Bottom