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No Smell, Quick and Easy, Almost Pure Bufotenine Extraction Options
 
soulfood
#201 Posted : 12/6/2012 10:48:10 PM

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Mindlusion wrote:
soulfood wrote:
the thing with acetic acid is it's a gas that is stabilized in water.

Citric acid and fumaric acid I nice convenient powders that are soluble in acetone so they're good to use.

The fumarate is way more stable than the freebase. Bufotenine freebase can go black in a matter of hours. I'd always store as a fumarate.


i think you may be thinking of carbonic acid, soulfood.

acetic acid is a carboxylic acid and quite stable. It can be a pure acid, a liquid with a fairly high melting point, and can be stored dry. (glacial acetic acid) You might be thinking of its reaction with sodium bicarbonate.



Righto.

I guess I was just thinking about that because it evaporates fully and I'm ignorant Smile

Looking back at my statement I can't even see how what I said about acetic would rule it out... liquid or gas.

I'm strange :s
 

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Mindlusion
#202 Posted : 12/7/2012 12:04:45 AM

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soulfood wrote:
Mindlusion wrote:
soulfood wrote:
the thing with acetic acid is it's a gas that is stabilized in water.

Citric acid and fumaric acid I nice convenient powders that are soluble in acetone so they're good to use.

The fumarate is way more stable than the freebase. Bufotenine freebase can go black in a matter of hours. I'd always store as a fumarate.


i think you may be thinking of carbonic acid, soulfood.

acetic acid is a carboxylic acid and quite stable. It can be a pure acid, a liquid with a fairly high melting point, and can be stored dry. (glacial acetic acid) You might be thinking of its reaction with sodium bicarbonate.



Righto.

I guess I was just thinking about that because it evaporates fully and I'm ignorant Smile

Looking back at my statement I can't even see how what I said about acetic would rule it out... liquid or gas.

I'm strange :s


heh well, actually when I look back at my original statement it doesn't make much sense to me today either. Very happy

--

but this thought has sparked some interest again to extract bufotenine.

What do we know about bufotenine in its natural state in the seeds, What do we know about its solubility in non-polar? My suspects are that its not, but for some reason its conflicting in my head....

If its not, it would be as simple as multi-defats with a good non polar like DCM, and a simple methanolic extraction to recover the alkaloids, with some hot and cold recrystallization. Acid/base isnt necessary
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"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Brennendes Wasser
#203 Posted : 6/19/2018 2:53:36 PM

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I now read most of the available TEKs for Bufo and now my remaining Question is:



Why CANT you just do a regular A/B ?


Well Bufo is too polar for Naphtha. But why can't you still do this:


1. Acidic cook of the Seed Powder (you will get Junk + Bufo Salt)

2. Basify it with NaOH to just slightly basic (~ pH Cool - with that CaCO3 you also won't get into much higher pHs so this step would be very similar (you will get Junk + Bufo FB)

3. Evaporate the water (it will not be too long, as you always have that small 50 g batches).

4. Pull with dry IPA or Acetone (you will get some Junk + FB)

5. Evaporate and purify with any Steps that are mentioned in those other TEKS (like the Acetone/Naphtha-Precipitation of the Junk).


Why won't this work ??

Thanks =)



EDIT: Why has nobody written anything on this or that other Bufo TEK thread since 5,5 years ? Oô
 
Loveall
#204 Posted : 6/19/2018 3:20:05 PM

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Hello. Your proposal is very similar to this wiki entry, which you may already be aware of. Do you toast the seeds to make the powder? After that your steps and the wiki steps look very similar, but there is no cleanup on the wiki Tek after the room temp IPA pulls.

Since the wiki Tek is expected to work, I would say your proposal is likely to work too. I would personally just follow the wiki as close as possible, that may be all that is needed. Not sure if you've tried that already.

One thing I would do try for fun is freezing cold quick IPA pulls (likely that has been already tired by someone?) that may give cleaner final pullls (?). I would compare that to the wiki tek results by pulling the wiki product with freezing IPA and testing what is left behind (if anything is) vs what is pulled by the cold IPA.
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Mindlusion
#205 Posted : 6/21/2018 3:30:00 AM

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Brennendes Wasser wrote:
I now read most of the available TEKs for Bufo and now my remaining Question is:



Why CANT you just do a regular A/B ?


Well Bufo is too polar for Naphtha. But why can't you still do this:


1. Acidic cook of the Seed Powder (you will get Junk + Bufo Salt)

2. Basify it with NaOH to just slightly basic (~ pH Cool - with that CaCO3 you also won't get into much higher pHs so this step would be very similar (you will get Junk + Bufo FB)

3. Evaporate the water (it will not be too long, as you always have that small 50 g batches).

4. Pull with dry IPA or Acetone (you will get some Junk + FB)

5. Evaporate and purify with any Steps that are mentioned in those other TEKS (like the Acetone/Naphtha-Precipitation of the Junk).


Why won't this work ??

Thanks =)



EDIT: Why has nobody written anything on this or that other Bufo TEK thread since 5,5 years ? Oô


What you are describing is not actually acid/base extraction, it is just an acid cook followed by a crude alcohol extraction. Acid base extraction is a liquid liquid extraction that involves moving the alkaloids from the aqueous phase to the non polar phase to purify it. So if you cook it in acid and then add base directly afterward, it doesn't really accomplish anything more than adding the base directly, especially if you going to dry it and extract it with alcohol afterward.

I would recommend toasting and grinding the seeds, defatting them with naphtha, making a paste with sodium carbonate, drying, then extracting with IPA or acetone.

The crude IPA or acetone extract is active. You can try to purify this resin through a/b extraction or recrystallization, but bufotenine freebase certainly has solublity problems in typical organic solvents. I never got a chance to try it back then, but I would try purifying the resin by salting it out of acetone with FASA. Perhaps by repeating that a few times, precipitating the freebase with sodium carbonate, you could get pure bufotenine.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Brennendes Wasser
#206 Posted : 6/21/2018 11:00:29 AM

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Yes its not actually an Acid / Base Extraction, but I just described it like this because it seems that this is the closest you can get to the standard A/B the guys here do for standard Spice, as there is no solvent to use as an organic pulling agent (because Bufo is only soluble in IPA + Acetone as far as I read and those wont separate from water of course).

So you said it would be somehow the same as freebasing it right from the beginning, but I just wonder if this first acidic cook may enhance yield, as you bring your Bufo into the same phase as you cook it with. If you do a basic cook, then most of the Bufo may get freebased, but as it is not soluble in water, maybe the efficiency is lower, as your cooking-solvent is not the phase in which the Bufo gets dissolved (of course it does not get dissolved at all, as you just have water + FB).

But what you say also sounds good, but as far as I read the purification of the FASA Salt converted to Freebase seems the best if you do this 1:4 Acetone:Naphtha precipitation, is this still the case ?


So possibly this would be good:

Toast Seeds
Grind Seeds
Defat with Naphtha
FB it with NaCO3 and dry
extract FB + Junk with Acetone/IPA
Precipitate with Fumarate
FB the Fumarate again
purify with that 1:4 Acetone/IPA:Naptha method

This is what I will try. Thanks so far, only some last Questions:


What temperature do you (MindLusion) use to roast the seeds? I am just asking everyone, because I really cannot imagine that a Temperature of 200°C + is not harmful. Do you also use that 240°C (which is 450°F as far as I understand) ? Also for how long ? Also do you roast it in a pan (then how do you check temperature ?! ;D) or in the oven ?

Also a second question:

It was stated that you could do another roasting on the FB Carbonate Seed Powder. But now Bufo is in the FB form and not the salt (which it should be within the seeds). Now it was also mentioned to do 200°C +. This sounds even more dangerous for me, as the FB should degrade much faster. Do you also do it or would you not recommend this additional cooking step?

Now the last question:

Whats the typical yield from like 100 g Seeds with your method ?


THXXX
 
Mindlusion
#207 Posted : 6/21/2018 3:06:34 PM

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Brennendes Wasser wrote:
Yes its not actually an Acid / Base Extraction, but I just described it like this because it seems that this is the closest you can get to the standard A/B the guys here do for standard Spice, as there is no solvent to use as an organic pulling agent (because Bufo is only soluble in IPA + Acetone as far as I read and those wont separate from water of course).

So you said it would be somehow the same as freebasing it right from the beginning, but I just wonder if this first acidic cook may enhance yield, as you bring your Bufo into the same phase as you cook it with. If you do a basic cook, then most of the Bufo may get freebased, but as it is not soluble in water, maybe the efficiency is lower, as your cooking-solvent is not the phase in which the Bufo gets dissolved (of course it does not get dissolved at all, as you just have water + FB).





Yeah I see what you were going for but in this case, because we are using IPA or acetone for the actual extraction, the acid boils will not make any difference at all, certainly none worth the time of adding and removing the water.

Brennendes Wasser wrote:



But what you say also sounds good, but as far as I read the purification of the FASA Salt converted to Freebase seems the best if you do this 1:4 Acetone:Naphtha precipitation, is this still the case ?


Yes that sounds good to me.

Brennendes Wasser wrote:


What temperature do you (MindLusion) use to roast the seeds? I am just asking everyone, because I really cannot imagine that a Temperature of 200°C + is not harmful. Do you also use that 240°C (which is 450°F as far as I understand) ? Also for how long ? Also do you roast it in a pan (then how do you check temperature ?! ;D) or in the oven ?

Also a second question:

It was stated that you could do another roasting on the FB Carbonate Seed Powder. But now Bufo is in the FB form and not the salt (which it should be within the seeds). Now it was also mentioned to do 200°C +. This sounds even more dangerous for me, as the FB should degrade much faster. Do you also do it or would you not recommend this additional cooking step?

Now the last question:

Whats the typical yield from like 100 g Seeds with your method ?


For roasting the seeds, I did them simply in a pan on low-medium heat. The seeds will expand and inflate as they remove steam, and sometimes pop like popcorn. This is a good indication when temperature is high enough, if it gets much hotter they will burn. Keep it like this until the inside seed colour changes from a light green to a more darker tannish brown. You can control the heat just by taking the pan on and off the burner as you go.

You could use the oven too, 200C+ sounds way too high. I would roast them the same way you roast walnuts, maybe putting them in the oven at 200F for 18 hours would be fine. But I never tried this.

Also, I would not roast the seed powder, just gently dry it and make sure the water is gone before going ahead with the extraction.

I don't have any real numbers but the yield is fairly low from what I can recall, a few hundred milligrams.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Brennendes Wasser
#208 Posted : 6/25/2018 9:46:15 PM

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Well I tried it and sadly I (as one may except as I am posting now) come back with some problems.


When I am at the step to throw in the Fumaric Acid, it looks very good as while pouring it in, I see big clouds crashing out. But then the solution simply keeps being cloudy, no precipitation of real material.

I tried to filter it through a coffee filter, but that does not do anything, it just runs through and nothing is left.


Now I read that someone just let this sit for the whole night and comes back to pour it off after this long waiting period. So does it really take that long to settle down?

I threw all my stuff away as I was not recovering any solid material from that stuff.

But do you guys also have experienced to simply wait at this salting step?

Or would it settle down directly as a solid mass, when you salt it ?


Again: There were extremely thick clouds crashing out, so at least this worked.
 
Mindlusion
#209 Posted : 6/25/2018 10:29:16 PM

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Brennendes Wasser wrote:

Now I read that someone just let this sit for the whole night and comes back to pour it off after this long waiting period. So does it really take that long to settle down?


Yes, it does. Normally I give it overnight, 12 hours, but full crystallization can take as long as 36 hours or more. You should have left it longer or stuck it in the fridge/freezer. At the beginning the crystals are microscopic and will fall through a filter, you must give them time to grow larger.

Brennendes Wasser wrote:


I threw all my stuff away as I was not recovering any solid material from that stuff.


Sad Never throw stuff away before you are sure. You threw away all the goodies.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Brennendes Wasser
#210 Posted : 7/4/2018 6:15:58 PM

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So I did it again and now I'm somewhere near to know if it all worked well or not : )

I just want to present a picture of my soup where I failed in the last run or at least where I thought I did.

It is right at this point:

Quote:
Add the contents of a 500 mg fumaric acid capsule directly to this solution and observe an instantaneous crashing out of bufotenine fumarate. This is a defatting step and effectively removes the plant oils and fats. Let this sit for a while to allow the reaction to complete. The bufotenine fumarate will stick to the sides and bottom of the jar and the waste acetone containing the unwanted oils can be poured off



So now something crashed out and it looks like this:




The brownish fluff is what I'm pretty sure is the precipitate, as it formed after the water got cloudy by adding Fumaric Acid and it appeared while the water was losing its cloudiness.
I separated both and placed the soup into the freezer, no further precipitates, so this must be the Fumarate salts.


I am simply asking here if this look familiar, as this does not really sound like the quote above. So please tell me if this look correct, after adding the Fumarate Salts to the Acetone-Pulls.

THXXX

(I have continued meanwhile and will check the end-result, my purification step with Acetone:Naphtha 1:4 is also done, but every junk crashed out at 1:1 already)
 
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