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TEK Ethyl acetate approach [CIELO]

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Hmm honestly I didn´t pay attention, I was trying to do a really quick extraction so I took some shortcuts, I didnt measure the amount of sodium carb so it was prob really concentrated solution, and after wash I decanted and just used it to extract straight away. If you use only a dilute solution and you freeze to remove excess water after, you´re prob not gonna have this issue in a significant way, but I think its important to keep in mind, a second water-only wash is a very simple addition to the work flow and would def prevent this issue.

if this does happen to anybody, sodium citrate is practically insoluble in alcohols including methanol, Im not sure mesc citrate solubility in ethanol or IPA, but its def soluble in methanol, so I separated it this way, soaking in methanol to dissolve mesc citrate and leave sodium citrate behind, but I have a rotovap to make sure no methanol is left when I evap it, I would avoid using it otherwise... But if mesc citrate is at soluble in IPA or ethanol one could use that instead.. Or just re-a/b and issue is solved. But better avoid it in the first place
 
So later I want to try cacti powder + CaCO3 and see if it also forms a nice paste (and try finding out if that gives a more-full-spectrum-extract or not)

So from what you say Ca(OH)2 works good, while Na2CO3 gives a bad consistency, unable to make the TEK easy.

Then what is this more of the origin: probably more the effect of the Ca(OH)2 which has the positive effect? Or the Na2CO3 which has the negative?

In case that it is only Na2CO3 which is bad (and not *only Ca(OH)2 which is good), did you also check if you can do:

cacti powder + NH3(aq)?

I think NH3 is terrible to work with, but just on a theoretical level it would also just freebase the alkaloids, but not phenolic OH- groups. So whatever would remain should still be a 'full spectrum' in the ethyl acetate.

I think these primary amines have the least basicity compared to secondary / tertiary, so NH3 would work still pretty good and not interfere with any R-OH.




And question #2:

If I want to try the benzoic acid / toluene way, would I just substitute the same moles? I guess as you try to precipitate mono-mescaline citrate it should be just the equimolar amount with benzoic acid?
 
Regarding washing and possible sodium citrate contamination; I had multiple cases where a small opaque third middle layer formed which i threw away with the bottom water layer. Only one case was this layer significant enough ~200mL that I saved it to try to recover. And it took a very long time (days) for the cloudiness to settle before i decanted again and froze and strained it but i never added it to my washed & dried EA for fear of unknowns.

Edit: woops :shock: i didn't realize there was a bunch of comments here previously on cloudy washed EA, I'll have to go take a closer read
 
Twilight Person said:
So later I want to try cacti powder + CaCO3 and see if it also forms a nice paste (and try finding out if that gives a more-full-spectrum-extract or not)

So from what you say Ca(OH)2 works good, while Na2CO3 gives a bad consistency, unable to make the TEK easy.

Then what is this more of the origin: probably more the effect of the Ca(OH)2 which has the positive effect? Or the Na2CO3 which has the negative?

In case that it is only Na2CO3 which is bad (and not *only Ca(OH)2 which is good), did you also check if you can do:

cacti powder + NH3(aq)?

I think NH3 is terrible to work with, but just on a theoretical level it would also just freebase the alkaloids, but not phenolic OH- groups. So whatever would remain should still be a 'full spectrum' in the ethyl acetate.

I think these primary amines have the least basicity compared to secondary / tertiary, so NH3 would work still pretty good and not interfere with any R-OH.




And question #2:

If I want to try the benzoic acid / toluene way, would I just substitute the same moles? I guess as you try to precipitate mono-mescaline citrate it should be just the equimolar amount with benzoic acid?
Click to expand...

Aomnia can react with ethyl acetate, I wouldn't use it.

Excess benzoic acid is fine, don't worry about moles. This is a lazy approach, just drop in about a teaspoon.
 
Hmmm so far not so good. Settled out the water and poured the solvent into a second vessel, added excess citric acid monohydrate and it clouded up. Goo was produced around the grains of citric acid at the bottom and agitation made no difference. I checked the PH and it was still alkaline so I assumed it was the trimescaline form. Adding extra citric acid didn't change anything. An addition of anhydrous citric acid just sat in a clump at the bottom and wouldn't dissolve.

I Rebased the precipitate again with lime after dissolving it in minimal water, pulled and settled for 24h in the fridge and used a pipette to draw off the solvent without any droplets. Added very finely ground citric acid monohydrate and made sure the PH was acidic. Now I have a cloudy solution with lots of goo droplets, no crystals so far.
 
It's been a good 5 hours, I'll wait and see for now.

A couple of ideas about this tek in general:

1: I personally would only use dried outer green flesh. There are a lot of impurities in the core and very little mesc.

2: Less material requires less solvent and you could save a lot this way.

3a: With a much smaller amount of material you could make a fully dried paste a couple of hours by fanning the cactus lime paste. This would save 24 hours in the fridge.

3b: This also eliminates the water variable from the base paste, as there isn't any added to begin with. Only bottled ethyl acetate is being used which usually has the right hydration level to begin with.
 
Orion said:
It's been a good 5 hours, I'll wait and see for now.

A couple of ideas about this tek in general:

1: I personally would only use dried outer green flesh. There are a lot of impurities in the core and very little mesc.
Click to expand...


I agree with many of your statements Orion. However what makes you say the core has impurities?

Using the core only yields the cleanest crystals (even without a wash) when using the Cielo tek. But your right it has very little mescaline. I found only 13% of what was in the green layer was found in the core. That new study posted recently seems to indicate there may be slightly more.
 
Orion said:
1: I personally would only use dried outer green flesh. There are a lot of impurities in the core and very little mesc.
Click to expand...

This research seems to show that although there is less mescaline, there is still mescaline to be had.

SOURCE: https://anoniem.org/?https://www.frontiersin.org/articles/10.3389/fpls.2023.1066595/full

FileProxy.ashx
 
Orion said:
Hmmm so far not so good. Settled out the water and poured the solvent into a second vessel, added excess citric acid monohydrate and it clouded up. Goo was produced around the grains of citric acid at the bottom and agitation made no difference. I checked the PH and it was still alkaline so I assumed it was the trimescaline form. Adding extra citric acid didn't change anything. An addition of anhydrous citric acid just sat in a clump at the bottom and wouldn't dissolve.

I Rebased the precipitate again with lime after dissolving it in minimal water, pulled and settled for 24h in the fridge and used a pipette to draw off the solvent without any droplets. Added very finely ground citric acid monohydrate and made sure the PH was acidic. Now I have a cloudy solution with lots of goo droplets, no crystals so far.
Click to expand...

Orion, sorry you are having this issue. I'm pretty sure we can figure this out, as many people are getting xtals reliably.

Side note: I'm a fan of your previous work on the nexus, thank you for that.

A few questions:

- Are you using the TEK ratios? If not what ratios did you use? I'm surprised your first salting was alkaline if you used the TEK ratios (they are designed to oversalt even the most powerful of cacti we have seen at 8%). You are correct that an alkaline extract will create goo instead of xtals.
- How long did you wait for the goo to change after adding more citric acid? It can take a while (days)
- I'm not very familiar with the mini A/B goo recovery, but it should have worked to first order. It is, however a different situation than when using the TEK, so I would not worry too much about it not working.
- Do you still have more cactus powder to try again depending on the answers above? It could simply be that you needed more citric acid added at the original salting step
 
Orion said:
It's been a good 5 hours, I'll wait and see for now.

A couple of ideas about this tek in general:

1: I personally would only use dried outer green flesh. There are a lot of impurities in the core and very little mesc.

2: Less material requires less solvent and you could save a lot this way.

3a: With a much smaller amount of material you could make a fully dried paste a couple of hours by fanning the cactus lime paste. This would save 24 hours in the fridge.

3b: This also eliminates the water variable from the base paste, as there isn't any added to begin with. Only bottled ethyl acetate is being used which usually has the right hydration level to begin with.
Click to expand...

1) In practice we have seen that spines/wax/core do not cause any issues in product purity or the process itself.
2) True, but the EA can be reused, so it is almost "free". There are some losses from solvent absorption, but the economics justify the extra mescaline in my opinion. I could be wrong though.
3) This is very tricky. Without water, lime particles diffuse into the EA wich are a pain do deal with. Even worse, the mescaline does not move well from a dried paste into the EA. I don't understand why, but experimentally I get little to no yield from a dry paste. Interestinly, if I re-wet the paste and pull again, I get normal yields. Some people say that dry mescaline freebase can salt itself in air with CO2 (?). I don't know, but I can say a fully dry paste does not yield well.
 
_Trip_ said:
Using the core only yields the cleanest crystals (even without a wash) when using the Cielo tek. But your right it has very little mescaline. I found only 13% of what was in the green layer was found in the core. That new study posted recently seems to indicate there may be slightly more
Click to expand...

I think your results is consistent with the paper. It can change from plant to plant and diameter of cut.

In my opinion it is reasonable to say that core gives a 10-20% boost to yields and worth using on the TEK when reusing solvent.

On the other hand, if I were drinking a bitter tea I would not add the core.
 
_Trip_ said:
I agree with many of your statements Orion. However what makes you say the core has impurities?
Click to expand...

I just mean anything that isn't mescaline but will go into your solvent. May not be too much of an issue with this tek though.

widderic, there definitely is some in there. I suppose it's personal preference. The paper mentions williamsii and pachanoi but I don't think I've seen much of an increase with the bridgesii I use. Personal preference I guess.

Speaking of volumes, I wonder if the concentration is the reason I've got goo instead of crystals ? I have used 400mg of mesc HCl and added water then lime to make a paste and pulled with about 100ml of Ethyhl Acetate. Perhaps this has behaved like spice when the naphtha is too concentrated, precipitating too quickly as a goo ? In the tek the solvent seems to be considerably less saturated before crystalizing. Perhaps that is the reason ? Just a guess.

I will try redissolving the goo in distilled water and evaporating to see if it crystalizes.
 
Orion said:
I will try redissolving the goo in distilled water and evaporating to see if it crystalizes.
Click to expand...
The TEK lists four options for dealing with goo:

(1) Do an A/B extraction on the goo,
(2) If a TEK execution is suspect, add the goo to cactus paste and do the TEK propely, increasing citric acid by the amount of expected mescaline present in the goo,
(3) decant off the solvent and cover the goo in fresh EA, it has been observed that crystals can grow out of the goo after a few days sitting in fresh solvent and stirring can help the process move along if crystal formation stops and there is still goo left, discard the solvent and add more
(4) if goo forms repeatedly, retry the TEK using fumaric acid instead of citric acid (fumaric may be more robust at forming xtals)


If you repeatedly get goo, try adding dry ethyl acetate to the extract before salting with citric acid. The theory being the additional EA will offset excess water in the extract.
 
Some hopefully useful info:
- Drying with K2CO3 is simple, effective and takes 10-20mins. So quicker than chilling and no extra work really than just decanting a second time.

- Conc. sulphuric acid can be used as well. Just add some drops of the acid to some ethyl acetate then add that to the dry ethyl acetate extract (dried with K2CO3). Pulls more colour with it though.

- Fumaric and tartaric acid both quickly form highly crystalline solids from dried ethyl acetate (dry with K2CO3). The fumarate and tartrate salts can be easily recrystallised from 95% ethanol. In both cases after recrystallisation there is a small amount of insoluble crystalline acid material (not the parent acid) and a small amount of brown impurity.

I’d love to take a look at a copy of the NMR files if someone can share them with me? I have topspin.
 
This tek select only mescaline from the cactus ? why ?

Is there a way to be more full spectrum, using a similar apoproach?


(asking to have a better / broader understanding before trying)
I'm exited to try pure mesc, but also in long term, i will probably want to extend to all alkaloids, as i truly beleive they are part of the magic :)
 
There is no evidence of a "full spectrum" alkaloids in significant quantities and effects in San Pedro, peruvianus and bridgesii. So far, other alkaloids have only been found in trace amounts in those 3 species. Even if they did, which there hasnt been a single publication showing it so far, it doesn't mean we could actually tell it apart if testing blind. Belief and self suggestion are way more powerful than people think.

Peyote and other cact like terscheskii may have other alkaloids in higher amounts, but afaik blind tests have not been done to show the significance of those alks in the effects.

My suggestion: regardless of this, give CIELO a try :)

Nemooo, Im attaching the .jdx NMR spectra, not sure if your software can open it.
 

Attachments

  • 1D_1H_20230209_003_284_Mescaline_II_203mg_IS-MA_297_corr.rar
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shroombee said:
Orion said:
I will try redissolving the goo in distilled water and evaporating to see if it crystalizes.
Click to expand...
The TEK lists four options for dealing with goo:

(1) Do an A/B extraction on the goo,
(2) If a TEK execution is suspect, add the goo to cactus paste and do the TEK propely, increasing citric acid by the amount of expected mescaline present in the goo,
(3) decant off the solvent and cover the goo in fresh EA, it has been observed that crystals can grow out of the goo after a few days sitting in fresh solvent and stirring can help the process move along if crystal formation stops and there is still goo left, discard the solvent and add more
(4) if goo forms repeatedly, retry the TEK using fumaric acid instead of citric acid (fumaric may be more robust at forming xtals)


If you repeatedly get goo, try adding dry ethyl acetate to the extract before salting with citric acid. The theory being the additional EA will offset excess water in the extract.
Click to expand...

I've done 1. 2 would mean harvesting cactus just for this. I'm only converting a small sample here so that would be a waste of time.

There seems to be no crystalization from dissolving the product in water and evaporating. From my understanding monomescaline citrate would crystalize from that, so if it doesn't then it must be trimescaline citrate or another form that somehow salted at an acidic PH. Not sure on that one.

3 will be the next one I try. As for 4... I already converted to HCL from fumarate before. I'm happier to return it to HCL. Easily done. By this point it will be the cleanest HCL I've ever seen :d

I wasn't just trying to see nice crystals but also get a product that was purity tested as just mescaline and not other alkaloids... which might not even be an issue now as endlessness says:

endlessness said:
There is no evidence of a "full spectrum" alkaloids in significant quantities and effects in San Pedro, peruvianus and bridgesii. So far, other alkaloids have only been found in trace amounts in those 3 species. Even if they did, which there hasnt been a single publication showing it so far, it doesn't mean we could actually tell it apart if testing blind. Belief and self suggestion are way more powerful than people think
Click to expand...

I've taken acetone-washed mesc HCL and had a quick comeup, early visuals and an easy come down. I've taken the equivalent dose of unwashed HCL and acetate mix and it felt as if it never came on until about 7 hours later when I hit a joint. It was both tiring and stimulating and had almost no open eyed visuals and strong closed eye visuals. Completely different experience. I'm sure I smoked a fat one after the first time too but it didn't do anything crazy. It's easy to understand why people believe how the unwashed or 'full spectrum' stuff is different. But like you say, there is no actual data. I'm divided on this, personally. It's like they have tested this cactus or that one, but what about mine :p ?

I can't argue that the data shows what the data shows.
 
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