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Lye/Limonene/Benzoic acid Options
 
Loveall
#21 Posted : 3/15/2022 1:54:11 PM

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Dasein wrote:
Loveall wrote:

- Salted limonene stirring in in 0.03 parts benzoic acid (this is new I believe). Extract became milky white as benzoic acid was dissolved.
- Small white xtals form (3rd picture). They where collected in a filter and washed with ethyl acetate (to remove limonene that can be difficult to evaporate). Dried on coffee filter with squeezing. Result is a white powder (4th picture). Will edit this post with results after collecting.


how did you add benzoic acid in limonene? dissolved in hot water? or directly in limonene? I read that benzoic acid is also soluble in hexane. If so, one could directly dissolve it in Naphtha to crash out DMT benzoate no?


Yes, I added the benzoic acid granules (3% by weight of root bark).

Yes, you can try to add benzoic acid to hexane, it should dissolve. As long as it reacts with DMT you will should get DMT benzoate to precipitate. I haven't tested that since with napthata I freeze precipitate to get FB.
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Dasein
#22 Posted : 3/15/2022 4:15:17 PM

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If DMT benzoate crystalizes that easily, it can be really great for pharma. Making Fumarate is not all that easy, you have to dry the acetone/IPA and then make sure it stays dry, and even then, water may get in during salting and keep the fumarate from crystalizing. I've had problems with that a couple of times, the salts didn't crystalize and I ended up with goo which wouldn't crystalize no matter what.
Getting benzoic acid could be a bit difficult, but it can be easily made from sodium benzoate and a strong acid right? I'll give it a try soon, this sounds pretty good!
این جهان با تو خوش است و آن جهان با تو خوش است
این جهان بی‌من مباش و آن جهان بی‌من مرو

ای عیان بی‌من مدان و ای زبان بی‌من مخوان
ای نظر بی‌من مبین و ای روان بی‌من مرو
 
Loveall
#23 Posted : 3/15/2022 6:35:58 PM

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Dasein wrote:
If DMT benzoate crystalizes that easily, it can be really great for pharma. Making Fumarate is not all that easy, you have to dry the acetone/IPA and then make sure it stays dry, and even then, water may get in during salting and keep the fumarate from crystalizing. I've had problems with that a couple of times, the salts didn't crystalize and I ended up with goo which wouldn't crystalize no matter what.
Getting benzoic acid could be a bit difficult, but it can be easily made from sodium benzoate and a strong acid right? I'll give it a try soon, this sounds pretty good!


Benzoic acid should be easy to get, was for me.

Success with limonene doesn't guarantee success with Naptha. Worth a test though. Good luck.

Also, if you are going for the salt, maybe Toluene/Benzoic acid is worth a test. Toluene should pull DMT better than naptha I believe. It is stinky though.
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shroombee
#24 Posted : 3/15/2022 7:57:08 PM

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Benzoic acid, cheap, and USP grade: https://www.amazon.com/gp/product/B07W6JQ7X9

I'm going to try this TEK maybe next week. I will report on the results.
 
Dasein
#25 Posted : 3/16/2022 7:53:41 AM

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Benzoic acid is not easily availble in europe, nor is limonene, but if anyone knows better... let me know!
این جهان با تو خوش است و آن جهان با تو خوش است
این جهان بی‌من مباش و آن جهان بی‌من مرو

ای عیان بی‌من مدان و ای زبان بی‌من مخوان
ای نظر بی‌من مبین و ای روان بی‌من مرو
 
Loveall
#26 Posted : 3/16/2022 10:33:19 AM

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shroombee wrote:
Benzoic acid, cheap, and USP grade: https://www.amazon.com/gp/product/B07W6JQ7X9

I'm going to try this TEK maybe next week. I will report on the results.


There is also amor_fati'sTEK that uses lime, but in step 12, scoop up some benzoic acid powder instead of doing the lab gear. Not sure if you need the CaCl2 step first.

Unless you grind lime very well you may see a drop in yields. Nice thing about lie is that it seems to help break down the bark, could be helpful with the larger fibers that are hard to grind.
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Loveall
#27 Posted : 3/16/2022 12:18:17 PM

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Ok, so I really like limonene after further testing. It pulls DMT free base well and doesn't saturated as easily as naphtha. Also, the FB in naphtha is temperamental in how it xtalizes. Therefore, I want to work on this approach more.

The whole point of a salt for me is making an e-juice with PG (propylene glycol). Want the e-juice to accept harmala salts too. A salt that may meet all these conditions is the acetate (we shall see).

So what would be an easy way to convert DMT benzoate from this TEK to DMT acetate? How about:

Wash with acetone. Dissolve DMT benzoate in minimal warm water and base with lime. Mix this with acetone, dry everything over CaCl2, decant, add white vinegar until no longer basic on pH paper, and dry to obtain DMT acetate.

If both DMT and Harmala acetate are soluble in PG I'm going to break out into a dance.
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iamalien
#28 Posted : 3/16/2022 12:24:51 PM
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Following this as want to try first d-limo extraction. Thank you for the encouragement!
 
shroombee
#29 Posted : 3/17/2022 4:25:19 AM

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Loveall wrote:
The whole point of a salt for me is making an e-juice with PG (propylene glycol). Want the e-juice to accept harmala salts too. A salt that may meet all these conditions is the acetate (we shall see).

So what would be an easy way to convert DMT benzoate from this TEK to DMT acetate? How about:

Wash with acetone. Dissolve DMT benzoate in minimal warm water and base with lime. Mix this with acetone, dry everything over CaCl2, decant, add white vinegar until no longer basic on pH paper, and dry to obtain DMT acetate

Wouldn't it be easier to use the Q21Q21 tek and get the DMT acetate directly?

I have 30/70 PG/VG e-liquid and some DMT acetate tincture. Is that useful for any tests?
 
Loveall
#30 Posted : 3/17/2022 9:26:46 AM

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shroombee wrote:
Loveall wrote:
The whole point of a salt for me is making an e-juice with PG (propylene glycol). Want the e-juice to accept harmala salts too. A salt that may meet all these conditions is the acetate (we shall see).

So what would be an easy way to convert DMT benzoate from this TEK to DMT acetate? How about:

Wash with acetone. Dissolve DMT benzoate in minimal warm water and base with lime. Mix this with acetone, dry everything over CaCl2, decant, add white vinegar until no longer basic on pH paper, and dry to obtain DMT acetate

Wouldn't it be easier to use the Q21Q21 tek and get the DMT acetate directly?

I have 30/70 PG/VG e-liquid and some DMT acetate tincture. Is that useful for any tests?


I think that Q21Q21 may not be very pure since evaporates water in bulk which can contain other stuff. I think a xtalization step is needed to get a cleaner product, but I could be wrong.

Yeah, that could be a test. I would dry a small sample of the tincture and see if it dissolves in the juice. If not all dissolves you could be looking at impurities depending on how you made the tincture. If all dissolves it would be a clear result.
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Loveall
#31 Posted : 8/27/2022 4:01:12 PM

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Loveall wrote:
shroombee wrote:
Loveall wrote:
The whole point of a salt for me is making an e-juice with PG (propylene glycol). Want the e-juice to accept harmala salts too. A salt that may meet all these conditions is the acetate (we shall see).

So what would be an easy way to convert DMT benzoate from this TEK to DMT acetate? How about:

Wash with acetone. Dissolve DMT benzoate in minimal warm water and base with lime. Mix this with acetone, dry everything over CaCl2, decant, add white vinegar until no longer basic on pH paper, and dry to obtain DMT acetate

Wouldn't it be easier to use the Q21Q21 tek and get the DMT acetate directly?

I have 30/70 PG/VG e-liquid and some DMT acetate tincture. Is that useful for any tests?


I think that Q21Q21 may not be very pure since evaporates water in bulk which can contain other stuff. I think a xtalization step is needed to get a cleaner product, but I could be wrong.

Yeah, that could be a test. I would dry a small sample of the tincture and see if it dissolves in the juice. If not all dissolves you could be looking at impurities depending on how you made the tincture. If all dissolves it would be a clear result.


Been thinking about this more.

Vaping dmt acetate is nice. Also, it could allow harmala acetate to be in an e-juice solution with it.

So how clean is a vinegar pull? I assumed the water would partition some unwanted stuff, but maybe that is wrong (?). Also, a brine wash before vinegar may make the acetate pure enough for vaping (?). Brine washes before salting are standard in lab workups, perhaps that extra cleanup step would help if not pure enough for vaping?

I think I'll start a separate work thread.
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Woolmer
#32 Posted : 10/26/2022 3:37:48 PM

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Loveall, why do you resort to a dry tek when using NaOH?

I pulled some A. Acuminata typical variant phyllodes with limonene (liquid-liquid, not dry tek). Salting with benzoic acid caused the formation of some chunks and a thin film over the glass that resulted to a goo when scraped. No crystals perhaps due to the messier nature of phyllodes.

6 mg of vaped dmt benzoate showed clear activity.
 
Loveall
#33 Posted : 10/26/2022 4:38:14 PM

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Woolmer wrote:
Loveall, why do you resort to a dry tek when using NaOH?

I pulled some A. Acuminata typical variant phyllodes with limonene (liquid-liquid, not dry tek). Salting with benzoic acid caused the formation of some chunks and a thin film over the glass that resulted to a goo when scraped. No crystals perhaps due to the messier nature of phyllodes.

6 mg of vaped dmt benzoate showed clear activity.


I wanted the least work possible, hence why dry tek. Used NaOH to break down the bark better.

Did you try to chemichaly dry the limonene before salting? Sometimes invisible water droplets with gunk are in there (they can also make the limonene cloudy). CaCl2 pellets should do it. It could be due to the different plant matter like you say, just wanna rule out water traces in the limo.
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Woolmer
#34 Posted : 10/26/2022 5:19:36 PM

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I did not try to chemically dry it. I will try to dry it with some MgSO4 on the next pull.
 
ymer
#35 Posted : 10/27/2022 1:37:12 AM

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Wait, so you can precipitate DMT from non-polar solvent directly by pouring the acid to the solvent?

This is the first time I hear this, I'm surprised no one else tried this before, why go through all the trouble of FASA or FASI if you can get clean crystals right out of the solvent and purify very easily after that? Surprised
 
Loveall
#36 Posted : 10/27/2022 2:26:02 AM

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ymer wrote:
Wait, so you can precipitate DMT from non-polar solvent directly by pouring the acid to the solvent?

This is the first time I hear this, I'm surprised no one else tried this before, why go through all the trouble of FASA or FASI if you can get clean crystals right out of the solvent and purify very easily after that? Surprised


It is acid in powder form. You dissolve the acid in the non polar and it reacts.

It is not trivial to find the right solvent/acid combo that will work. If using naphtha FASA is needed as I'm not aware of any acid that dissolves directly in naptha. Benzoic acid dissolves in limonene and it reacts to precipitate the salt. Note that we have not analyzed dmt benzoate candidate yet.

However, add benzoic acid to ethyl acetate containing mescaline FB and while it dissolves it won't precipitate salt. On the other hand add citric acid and it will react and form very pure mescaline monocitrate. If you try citric acid with dmt FB in Ethyl acetate you get a goo. Etc ,etc.

We are trying to document all the good combos for our favorite molecules.
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ymer
#37 Posted : 10/27/2022 2:39:18 AM

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Loveall wrote:
It is acid in powder form. You dissolve the acid in the non polar and it reacts.

It is not trivial to find the right solvent/acid combo that will work. If using naphtha FASA is needed as I'm not aware of any acid that dissolves directly in naptha. Benzoic acid dissolves in limonene and it reacts to precipitate the salt. Note that we have not analyzed dmt benzoate candidate yet.

However, add benzoic acid to ethyl acetate containing mescaline FB and while it dissolves it won't precipitate salt. On the other hand add citric acid and it will react and form very pure mescaline monocitrate. If you try citric acid with dmt FB in Ethyl acetate you get a goo. Etc ,etc.

We are trying to document all the good combos for our favorite molecules.


I see.

As someone stated before, benzoic acid dissolves in hexane, and I have access to hexane and benzoic acid, so I will give it a try as soon as I can and post my results.
 
Woolmer
#38 Posted : 10/27/2022 9:14:34 AM

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Drying with MgSO4 did clear up the limonene considerably, though the result is mostly the same after salting. But goo is not the right term it is more waxy/solid and not difficult to handle. I have yet to wash the trace limonene and I suspect this might be what is keeping it waxy and preventing it from hardening up nicely. Liking this tek a lot Thumbs up
 
tryptamine9
#39 Posted : 10/27/2022 9:27:13 AM

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Dasein wrote:
Benzoic acid is not easily availble in europe, nor is limonene, but if anyone knows better... let me know!


I had absolutely no trouble buying benzoic acid online here in EU.
It has a variety of uses as it inhibits groth of fungi and bacteria.
 
Loveall
#40 Posted : 10/27/2022 12:36:54 PM

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ymer wrote:
Loveall wrote:
It is acid in powder form. You dissolve the acid in the non polar and it reacts.

It is not trivial to find the right solvent/acid combo that will work. If using naphtha FASA is needed as I'm not aware of any acid that dissolves directly in naptha. Benzoic acid dissolves in limonene and it reacts to precipitate the salt. Note that we have not analyzed dmt benzoate candidate yet.

However, add benzoic acid to ethyl acetate containing mescaline FB and while it dissolves it won't precipitate salt. On the other hand add citric acid and it will react and form very pure mescaline monocitrate. If you try citric acid with dmt FB in Ethyl acetate you get a goo. Etc ,etc.

We are trying to document all the good combos for our favorite molecules.


I see.

As someone stated before, benzoic acid dissolves in hexane, and I have access to hexane and benzoic acid, so I will give it a try as soon as I can and post my results.



Oh, yeah, I had that wrong. There is some solubility of benzoic acid in naphtha. Interesting.
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