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Ethyl acetate approach [CIELO] Options
 
famine
#1361 Posted : 3/17/2023 1:44:54 PM

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endlessness wrote:
famine wrote:
]
Dry your ethyl acetate before freezing just... Shocked


This was tried already before by Loveall and others and drying your ethyl acetate with magnesium sulphate for example will interfere with crystallization and result in lower yields. One possibility is that the mescaline citrate is crystallized as monohydrate and it needs some of the extra water for proper crystallization, so a fully dried solvent isnt wanted in this case. I haven´t tested this in a side by side experimentally (would of course be interested if anybody does) but I have extracted and crystallized mescaline several times now with the Ethyl acetate containing water within these acceptable ranges and it works perfectly. As they say, don´t change a winning team Very happy

Orion wrote:
Well... this thread took forever to read through but it was worth it. There is some seriously thorough work in these pages! I'll definitely be trying this.

Endlessness, nice crystal assortment. You mentioned freezing and I wonder: could the ethyl acetate not be poured away from the ice ? Is there a reason to allow it to thaw first ?

EDIT: For the sake of growing crystals for fun before any harvests, what would be a good way to test converting HCl to citrate using this method ? Half a gram for example. Add water, base with lime, dry, pull with ethyl acetate and proceed as normal ?


Orion, I didnt pour away/filter the ice because I didn´t want to remove too much water that potentially would interfere with crystallization later on. Also I am not sure of the solubility of mescaline in Ethyl Acetate at freezing temperatures so I was worried that some of the mescaline might have separated from ethyl acetate and be filtered away. One could of course test this easily experimentally but I didn´t want to do a side by side, I just wanted to make sure I got all my mescaline in a short time, so I figured that would be the easiest way.

And yeah I think you could convert your HCl to citrate that way. If you add just enough water for the HCl to dissolve, when you add lime it will already be quite dry so you can pull with ethyl acetate straight away without having to dry it. And a bit of extra water shouldn´t be a problem in any case as mentioned above, specially if you do a fridge (or quick freeze and thaw) step to get the water content to that acceptable range.

Perhaps the water crystals act as points of nucleation. One must try having a dry concentrated solution of mescaline citrate in EtOAc, scratch the glass up alot and freeze!
 

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Loveall
#1362 Posted : 3/17/2023 2:29:25 PM

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As endlessness said, EA works great with water from the fridge rest. So far, experimental chemical drying is extra work for no benefits and causes possible issues.

If someone really wants to avoid water in the solvent, they can try a toluene/benzoic acid system (CITLO). This may be even less work than CIELO since the fridge rest may not be required. However Toluene is not food safe and (for my taste) less pleasant to work with.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
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πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
famine
#1363 Posted : 3/17/2023 2:59:14 PM

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Toluene definitely not an option here if we are trying to make an easy TEK for the common kitchen chemist.
 
Orion
#1364 Posted : 3/17/2023 3:56:24 PM

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Wouldn't the lack of water in the toluene cause an issue though ? If my understanding is correct, the small amount of water in ethyl acetate is actually helpful.

About the citric acid, would it be best to use the monohydrate form rather than anhydrous ?
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Loveall
#1365 Posted : 3/17/2023 4:51:21 PM

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Orion wrote:
Wouldn't the lack of water in the toluene cause an issue though ? If my understanding is correct, the small amount of water in ethyl acetate is actually helpful.

About the citric acid, would it be best to use the monohydrate form rather than anhydrous ?


Toluene and benzoic acid work great without any water. Mescaline benzoate xtalizes very well in toluene. As a side note - mescaline benzoate did not xtalize from EA πŸ€·β€β™‚οΈ

Both anhydrous and monohydrate citric acid work well with the TEK. This is because EA has ~2.5% water when salting which will overwhelm the citric acid initial condition. Note that there seems to be a difference in solubility bewteen ctiric acid hydrate forms when using dry EA, but the TEK avoids that.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
endlessness
#1366 Posted : 3/17/2023 5:31:10 PM

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From my experience I highly recommend monohydrate citric acid instead of anhydrous, the anhydrous did not dissolve well at all even with a lot of stirring and even ultrasonic bath. Not sure why that happened if the EA after pulling has some water content, and if others were able to make it work but for me it only worked well using anhydrous citric acid if i predissolved it in ethyl acetate that I added enough water to, and then added that to the ethyl acetate pulls
 
Twilight Person
#1367 Posted : 3/17/2023 5:54:09 PM

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Quote:
Toluene and benzoic acid work great without any water. Mescaline benzoate xtalizes very well in toluene. As a side note - mescaline benzoate did not xtalize from EA πŸ€·β€β™‚οΈ


So it works great for crystallization, but does it also behave the same with the cactus paste? Like is there the same performance when I add the foluene to my paste like Ethyl Acetate or was this never tested, just if I could get crystals when already starting with pure mescaline?

I would try that benzoic / toluene way maybe in future, but first will need to wait for my poor cactus to suffer a little more in darkness.
~ O ~
 
Loveall
#1368 Posted : 3/17/2023 6:26:48 PM

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endlessness wrote:
From my experience I highly recommend monohydrate citric acid instead of anhydrous, the anhydrous did not dissolve well at all even with a lot of stirring and even ultrasonic bath. Not sure why that happened if the EA after pulling has some water content, and if others were able to make it work but for me it only worked well using anhydrous citric acid if i predissolved it in ethyl acetate that I added enough water to, and then added that to the ethyl acetate pulls


How long did you wait for anhydrous citric acid to dissolve in the extract? Eventually it will dissolve in my experience, but 24h of "hydration" in wet EA may be necessary. Also, with a lot agitation mescaline citrate crashes as a powder (instead of needles) that can look like citric acid.

I would expect 2.5% wet EA to dissolve anhydrous citric acid both for EA extracts and CASEA prep. Haven't tested CASEA, but it has worked on extracts.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Loveall
#1369 Posted : 3/17/2023 6:29:26 PM

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Twilight Person wrote:
Quote:
Toluene and benzoic acid work great without any water. Mescaline benzoate xtalizes very well in toluene. As a side note - mescaline benzoate did not xtalize from EA πŸ€·β€β™‚οΈ


So it works great for crystallization, but does it also behave the same with the cactus paste? Like is there the same performance when I add the foluene to my paste like Ethyl Acetate or was this never tested, just if I could get crystals when already starting with pure mescaline?

I would try that benzoic / toluene way maybe in future, but first will need to wait for my poor cactus to suffer a little more in darkness.


Needs to be tested starting with powder/paste. Unpublished reports sound promising.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
starbob
#1370 Posted : 3/17/2023 8:07:03 PM

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endlessness wrote:
So when trying to dissolve anhydrous citric acid in ethyl acetate, I added 11.1g anhydrous citric acid in 250ml ethyl acetate. It did not dissolve much at all, even after overnight stirring in a magnetic stirrer and some time in the ultrasonic bath.

So I decided to add water in small amounts until it all dissolved. It took about 5ml water for the citric acid to dissolve completely.


I thought I'd mention this same ratio worked perfectly for me with Milliard's food grade anhydrous CA. ~0.5mL distilled water per gram of anhydrous citric acid.

I was only going for 25mg/mL CA:EA, not a maximum concentration true saturate. I added 1mL water at a time on mag stirrer. I used ~300mL fresh ethyl acetate, ~7.5g citric acid, & ~4mL distilled water (only because I couldn't really do smaller increments than 1mL with my equipment at the time).
 
Orion
#1371 Posted : 3/18/2023 12:26:50 AM

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Am I right in thinking that no matter which form of citric acid is used, the same compound will form, not a different one with a different level of hydration and possibly a different potency ?

Just making sure as I do have both anhydrous citric acid and the monohydrate.
Art Van D'lay wrote:
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Loveall
#1372 Posted : 3/18/2023 1:15:36 PM

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Orion wrote:
Am I right in thinking that no matter which form of citric acid is used, the same compound will form, not a different one with a different level of hydration and possibly a different potency ?

Just making sure as I do have both anhydrous citric acid and the monohydrate.


I think you get the same result because of the water in EA.

Endlessness recommended the monohydrate because it dissolves more easily so you can choose that.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Toshido
#1373 Posted : 3/18/2023 3:30:00 PM

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Loveall wrote:

Endlessness recommended the monohydrate because it dissolves more easily so you can choose that.


Yeah I ended up finding out that my citric acid is Anhydrous Sad . I'll just get a different brand.
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Loveall
#1374 Posted : 3/18/2023 4:32:04 PM

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widderic wrote:
Loveall wrote:

Endlessness recommended the monohydrate because it dissolves more easily so you can choose that.


Yeah I ended up finding out that my citric acid is Anhydrous Sad . I'll just get a different brand.


It should work in my experience. Just takes a while to dissolve, but it will dissolve for me.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
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endlessness
#1375 Posted : 3/18/2023 5:23:05 PM

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Widderic you can just do the 'trick'I described earlier which also worked for starbob, to predissolve the citric acid in fresh EA with a bit of water and then add that to your mesc EA pulls, no need to buy another citric acid
 
endlessness
#1376 Posted : 3/18/2023 6:47:51 PM

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Btw Loveall, _Trip_ and others, did you ever by any chance check the solubility of mesc citrate in ethanol, isopropanol, water and other solvents?
 
Loveall
#1377 Posted : 3/18/2023 8:44:11 PM

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endlessness wrote:
Btw Loveall, _Trip_ and others, did you ever by any chance check the solubility of mesc citrate in ethanol, isopropanol, water and other solvents?


Found it slowly soluble in water (did not measure) and mostly insoluble in e-juice (PG/VG).
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
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Twilight Person
#1378 Posted : 3/19/2023 9:13:40 PM

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If you would completely evaporate the Ethyl Acetate at the end how much material is retrieved upon?

Is it nearly nothing so you just extract mescaline and precipitate basically everything? Or will you have some oils/fats/other alkaloids at the end inside of that EA?
~ O ~
 
endlessness
#1379 Posted : 3/19/2023 9:42:25 PM

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This is a test I was meant to do but ended up skipping it for now.. I´ll def do at some point, evap the ethyl acetate and see what is left there.
 
cyantific
#1380 Posted : 3/21/2023 5:37:49 AM

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With full spectrum tea, cacti species plays a big part of the experience… with CIELO would you be able to tell difference?
 
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