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ACRB extraction with acetone+FASA went wrong Options
 
reddog
#1 Posted : 4/7/2015 2:23:45 PM

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So, I have had good experience with bufotenine extraction using only acetone as a solvent. Since, I haven't had any other solvents at hand, I attempted an analogous ACRB extraction. Mostly, the beginning is Q21Q21's dry tek with lime.

The following has been done:

1. Grind 10g of ACRB into fine rose-colored powder
2. Add enough 20% acetic acid to make the powder wet (~20ml)
3. Add enough water to make the mix flow (~50ml)
4. Mix thoroughly and let it sit for 40 min
5. Add ~10g lime, yielding a brown-gray crumbly paste
6. Mix for 10 min and let it sit for 5 hours

From here I digressed from the tek, because I wanted to use acetone to pull and salt with FASA.

7. Dry the mix in an oven at 50-70°C (it was already quite dry, but I made sure pretty much all water was gone)
8. Put the mix into The Herbal Percolator (THP) and pull 10 times with the same 500ml acetone -> The acetone came out almost unchanged color-wise
9. Add some drops FASA to the resulting acetone -> Nothing happened, at all, no clouding observed

At this point, I was pretty sure, I messed up something. Still, I evapped all the acetone and was left with a very small amount of nicely smelling oil (smelled a bit sweet and a bit like Sandalwood perfume). It was about 20mg oil. I tried evaporating a drop over tin-foil without any effect.

Can someone help me to find my mistake? I know, that it's not a wise move to digress from a working tek. This is why I tried with just 10g. Still, I wonder, why it has not worked? Was this just too little material? Was is too much acid, so the lime couldn't base it enough? Was it too little time for basification?

From what I know about DMT solubility in acetone, it should be perfectly possible to pull free-base with acetone.

Thanks for any help.
 

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endlessness
#2 Posted : 4/7/2015 2:41:30 PM

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Maybe try again without the acetic acid, and also I'd try adding some more calcium hydroxide, see if it helps.

I've tried something similar but using sodium carbonate and mimosa, and it didnt work well, the alkaloids did not precipitate, possibly due to impurities keeping the alkaloids from precipitating. Maybe if nothing precipitates, the resulting product can again be based and pulled again (and the pull filtered to remove inactives), and precipitated again, could yield something purer.

Im neither sure how the NMT situation will change the fumarate crystallization, since I havent yet worked with acacia extractions.

Either way, do keep us updated on any further experiments, and good luck!
 
reddog
#3 Posted : 4/7/2015 7:15:53 PM

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Thank you, Endlessness.

I'm trying to add more lime to the mix, right now. Don't have much hope, though. I might experiment again, with another 10g. On the other hand, maybe I'm just gonna brew some Aya from it instead ^^ OR wait until I can afford some limonene. Too bad, I'm not in the US. Limonene seems to be quite cheap in the States.
 
reddog
#4 Posted : 4/7/2015 10:34:16 PM

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Man, chemistry just drives me crazy xD

I added another 10g lime as I said. Added enough water to make a paste and dried it completely, again. Put that into THP with 300 ml acetone. What I got is...

JELLO! What the... I've never seen jello forming out of acetone <(o.O< )

It is transparent jelly-like substance which sticks to the walls and the bottom of the container. Does anyone has ANY idea what this might mean? I'm afraid, don't ^_^
 
endlessness
#5 Posted : 4/7/2015 11:24:00 PM

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What material is your THP made of? Plastic and acetone is generally not good mix.

If it's not plastic, I'd just evap it all and see what you have left. Then try to base and re-FASA it, see what happens
 
pitubo
#6 Posted : 4/8/2015 12:00:41 AM

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reddog wrote:
Man, chemistry just drives me crazy xD

I added another 10g lime as I said. Added enough water to make a paste and dried it completely, again. Put that into THP with 300 ml acetone. What I got is...

JELLO! What the... I've never seen jello forming out of acetone <(o.O< )

It is transparent jelly-like substance which sticks to the walls and the bottom of the container. Does anyone has ANY idea what this might mean? I'm afraid, don't ^_^

1. Calcium hydroxide plus acetic acid makes calcium acetate, a substance that forms a gel in combination with ethanol, perhaps also to an extent with acetone.

2. Acetone plus base (calcium hydroxide is a base) plus heat plus time = acetone self-condensation, forming (among others) mesityl oxide. I guess using acetone in the herbal percolator to extract alkaline (and acidic too) matter is not advisable.
 
reddog
#7 Posted : 4/8/2015 7:02:15 AM

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My THP is made from a glass bottle. And it worked fine with bufotenine extraction, though I used sodium carbonate+acetone there.

I evapped the gel which has not stuck to the cotton. It gave a considerable amount of oil. Smells the same as the one from the first pull. It did dry somewhat over night, so I'll let it dry completely and see if I can base it again. It's very little dry material, but I started with just 10g ACRB, so no surprise.

Seems that acetone pulls too much additional material which prevents the product from reacting with fumaric acid. Too bad.
 
reddog
#8 Posted : 4/8/2015 1:13:07 PM

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I think I'm going to try Infundibulum's "abandoned" tek

I don't see, how 200ml acetone per 10g of bark is too expensive. I still have 5l from my 10l canister left. CASA/FASA sounds like a nice intoxic approach. I'm not sure, how exactly the product is extracted in step 2 in the first place. Isn't it trapped inside the cells? Or are they destroyed sufficiently by the powdering process?
 
reddog
#9 Posted : 4/10/2015 8:00:17 AM

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Latest update:
I have let the oily stuff dry completely, yielding ~200mg of yellow substance that smells sweet. I then mixed it with sodium carbonate and made a paste with water. Let this dry completely over night, then made a powder and mixed it with acetone. Filtered through a cotton ball, yielding almost clear acetone. Added a couple of drops of FASA. Nothing happened, no clouding. Momentarily, I let it sit for 8-9 hours. I'll check on it later, maybe something will precipitate eventually.

However, I assume there's just not much alkaloid in there.
 
 
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