TEK Ethyl acetate approach [CIELO]

[Loveall]

Thanks endlessness/BW.

Could there simply be water in the xtaline structure? Could the product simply be monomescaline citrate (mono/di)ydrate?

For example how would the NMR look for mescaline sulfate dihydrate? Can you see a difference between water "contamination" and water as part of the natural salt?

Hydrate xtals molecules can have half a molecule of water (shared), so perhaps the product we are looking at is,

Mes(↑) + H3Cit(↑) + 1.5H2O ⇒ (MesH)H2Cit·1.5H2O(↓)​

With the notation mentioned in the Wiki. This matches endlessness' result result of 49% mescaline.

Would need repeat of the NMR results and verify that the water is not a contaminant.

I've tentatively updated the xtalization precipitation reaction in the WIKI to this.

The hydration would imply that instead of 61% as strong as MesHCl by weight, our product is 57% as strong.

 

[Twilight Person]

I see all traditional methods use Ca(OH)2.

But why we dont use Na2CO3?

It is a weaker base and also strong enough for Mesc I guess?

But maybe it will not deprotonate the HO-R Alkaloids and it looks like there are quite many in those cacti. Maybe then the spectrum and experience would be more enriched, like what people claim for cactus tea?

Ca(OH)2 has a pretty bad solubility in water, is that important? Other than that I see no real difference, just carbonates being weaker bases.

 

[Loveall]

I see all traditional methods use Ca(OH)2.

But why we dont use Na2CO3?

It is a weaker base and also strong enough for Mesc I guess?

But maybe it will not deprotonate the HO-R Alkaloids and it looks like there are quite many in those cacti. Maybe then the spectrum and experience would be more enriched, like what people claim for cactus tea?

Ca(OH)2 has a pretty bad solubility in water, is that important? Other than that I see no real difference, just carbonates being weaker bases.

Paste made with Na2CO3 becomes gooey quickly and is not loose/sandy. Makes it hard for the ehtyl acetate to get into the paste and extract mescaline effectively.

 

[Twilight Person]

Ok I see!

Now when comparing both the really low solubility of Ca-Salts comes in mind.

Is there any chance to try it with CaCO3?

If that shares the same consistency with Ca(OH)2 then maybe could be an option to keep more actives?

 

[Loveall]

Ok I see!

Now when comparing both the really low solubility of Ca-Salts comes in mind.

Is there any chance to try it with CaCO3?

If that shares the same consistency with Ca(OH)2 then maybe could be an option to keep more actives?

Maybe? I don't know. I would worry it may not give a high enough pH. I never tried it but you can if you want.

 

[Toshido]

How can I tell if my Citric Acid is Monohydrate or Anhydrous? Any way to tell without testing it with Ethyl Acetate? I have some citric acid but it doesn't specify.

Also, is food grade Calcium Hydroxide (pickling lime) ok to use?

 

[Loveall]

It doesn't matter if the citric acid is anhydrous. This is because there will be 2.5% water after the fridge rest, and that will wet anhydrous acid if present (may take a little longer to dissolve).

Food grade Calcium Hydroxide is good to use

 

[Toshido]

It doesn't matter if the citric acid is anhydrous. This is because there will be 2.5% water after the fridge rest, and that will wet anhydrous acid if present (may take a little longer to dissolve).

Food grade Calcium Hydroxide is good to use

Thank you. I saw that Endlessness used CASEA (Citric Acid Saturated Ethyl Acetate) that he simply added to his pulls. So I guess I will just test it out first.

 

[Loveall]

It doesn't matter if the citric acid is anhydrous. This is because there will be 2.5% water after the fridge rest, and that will wet anhydrous acid if present (may take a little longer to dissolve).

Food grade Calcium Hydroxide is good to use

Thank you. I saw that Endlessness used CASEA (Citric Acid Saturated Ethyl Acetate) that he simply added to his pulls. So I guess I will just test it out first.

If you want to use CASEA, then it does matter. When preparing CASEA using dry entyl acetate and anhydrous citric acid you may need to add 2% water to get the citric acid to dissolve.

 

[Toshido]

If you want to use CASEA, then it does matter. When preparing CASEA using dry entyl acetate and anhydrous citric acid you may need to add 2% water to get the citric acid to dissolve.

Oh ok great thanks for letting me know in case I run into that issue. As for dry ethyl acetate... what makes it.... dry? As I am using MEK Substitute as stated in the TEK which is 100% ethyl acetate.

 

[Loveall]

If you want to use CASEA, then it does matter. When preparing CASEA using dry entyl acetate and anhydrous citric acid you may need to add 2% water to get the citric acid to dissolve.

Oh ok great thanks for letting me know in case I run into that issue. As for dry ethyl acetate... what makes it.... dry? As I am using MEK Substitute as stated in the TEK which is 100% ethyl acetate.

It is pretty dry out of the can. If exposed to water it reaches equilibrium at ~3% water at room temp and ~2.5% at fridge temp. After it absorbs water it can be dried again by one of several methods, but that is not needed for this TEK.

 

[Toshido]

It is pretty dry out of the can. If exposed to water it reaches equilibrium at ~3% water at room temp and ~2.5% at fridge temp. After it absorbs water it can be dried again by one of several methods, but that is not needed for this TEK.

So free of water, makes sense. Thank you for clarifying! My brain is swollen from all of the learning in the last few months haha. Not a bad thing.

 

[endlessness]

Got my best yield yet, 2.4% !

It was from a mix of cact (whole cact, spines, core and all), there was maybe 70% of some cact I had extracted from before and had gotten 1% yield, but it was a couple of pieces that were cut during winter and didn´t heal/scar properly so they were rotting near the cut.. The other 30% was a bridgesii I hadnt extracted before. So either rotting cact creates more mesc and/or my bridgesii has a crazy high yield...

Also, it was with reused ethyl acetate, and I made the whole extraction in like 10 mins of work plus some waiting, was crazy simple and easy.

I also didn´t want to wait for the fridge step overnight duration so what I did instead is to put the ethyl acetate in the freezer for a couple of hours until there was some frozen water slush in the ethyl acetate, then I took it out of the freezer and let it stand in room temperature for half an hour or so until the ice slush had melted and there was a water puddle on the bottom of ethyl acetate, so I just decanted the ethyl acetate away from that and used to make the pulls.

I did very quick pulls and then crystallized by dumping Citric Acid Saturated Ethyl Acetate (CASEA) that had about 10g citric acid into the 1L mescaline-laden ethyl acetate and let it crystallize overnight. Prob because of the reused ethyl acetate I got a mix of different types of crystals, some fluffy needles mixed with some more amorphous crystals, as seen below:

 

[famine]

Got my best yield yet, 2.4% !

It was from a mix of cact (whole cact, spines, core and all), there was maybe 70% of some cact I had extracted from before and had gotten 1% yield, but it was a couple of pieces that were cut during winter and didn´t heal/scar properly so they were rotting near the cut.. The other 30% was a bridgesii I hadnt extracted before. So either rotting cact creates more mesc and/or my bridgesii has a crazy high yield...

Also, it was with reused ethyl acetate, and I made the whole extraction in like 10 mins of work plus some waiting, was crazy simple and easy.

I also didn´t want to wait for the fridge step overnight duration so what I did instead is to put the ethyl acetate in the freezer for a couple of hours until there was some frozen water slush in the ethyl acetate, then I took it out of the freezer and let it stand in room temperature for half an hour or so until the ice slush had melted and there was a water puddle on the bottom of ethyl acetate, so I just decanted the ethyl acetate away from that and used to make the pulls.

I did very quick pulls and then crystallized by dumping Citric Acid Saturated Ethyl Acetate (CASEA) that had about 10g citric acid into the 1L mescaline-laden ethyl acetate and let it crystallize overnight. Prob because of the reused ethyl acetate I got a mix of different types of crystals, some fluffy needles mixed with some more amorphous crystals, as seen below:

Dry your ethyl acetate before freezing just... :shock:

 

[Orion]

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 ?

 

[Quetzal7]

I'm getting ready to try that tek soon =) =)

Question : did anybody tried to put fresh cactus in the blender and add to lime to it directly?

I remember adding lime to dry cactus powder (Q21 tek kind of approach) and making the opposite as what is describes here : it got goey really really fast, but 2 days after, the texture changed completly and it was sandier (but not sandy sandy, still has some elasticity to it)

While , as a test, i put fresh cactus in the blender and lime, it was much much better texture imho =)
(but i didn't tried to pull, it was just information... you know... casuality making cactus-lime smoothies with the vitamix... )

 

[endlessness]

]
Dry your ethyl acetate before freezing just... :shock:

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

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.

 

[famine]

]
Dry your ethyl acetate before freezing just... :shock:

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

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!

 

[Loveall]

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.

 

[famine]

Toluene definitely not an option here if we are trying to make an easy TEK for the common kitchen chemist.