IPA and ammonia

[Loveall]

See attached document, mentioning that warm alcohol + ammonia extracts mescaline from plants (along with other stuff). Starting from that point I wonder if we could try something like this (has it been mentioned/tried before?)

- Extract dry cactus powder with warm 99% alcohol and drops of 10% ammonia (just enough to get to pH 11.5 after reacting with plant-stuff). Want to minimize excess water.
- Titrate with HCl. Solubility of NH4Cl in IPA is 180mg/100ml (ref) so that salt should stay in solution (up to a point).
- Hope that mescaline HCl crashes out (other stuff may also crash). Decant/Filter precipitate.
- Wash with IPA to clean up.

It would be a fantasy come true if it works (so it probably won't )

If anyone knows why this would not work that info would be very welcome. Any feedback welcome too. I may give this a shot if it has indeed not been tried yet and seems viable. Cheers.

 

[doubledog]

I have extracted dry cactus with ammonia alcohol
-first pull 95% IPA + 5% ammonia water
-second pull 99% IPA,
-liquid combined, evaporated to dryness,
-Dissolved in acidic water
-filtered
-again evaporated to resin.
The resin was fully active.

There is still lot of other stuff in the extract, so mescaline is not the molecule with the highest concentration. I would say these other compounds prevent crashing of mescaline, it seems to increase its solubility.

 

[Loveall]

I have extracted dry cactus with ammonia alcohol
-first pull 95% IPA + 5% ammonia water
-second pull 99% IPA,
-liquid combined, evaporated to dryness,
-Dissolved in acidic water
-filtered
-again evaporated to resin.
The resin was fully active.

There is still lot of other stuff in the extract, so mescaline is not the molecule with the highest concentration. I would say these other compounds prevent crashing of mescaline, it seems to increase its solubility.

Thanks, this is great info How much final resin did you get (vs expected mescaline amount)? Did you try to wash the resin with 99% IPA or clean it up further in any way?

 

[doubledog]

Yes, tried to wash it with IPA and also tried to crash the mescaline from water solution by addition of IPA (hcl was used as acid). No success.

My findings are that these remaining inactive compounds have very similar solubility as mescaline salts - are soluble in water, insoluble in IPA. But this insolubility is not absolute, something goes through.

Another pH change to freebase is needed.

This resin is excellent for proceeding to A/B with use of NPS.

 

[Loveall]

...tried to crash the mescaline from water solution by addition of IPA (hcl was used as acid). No success.

No success because both the mescaline and other salts crashed or no success because nothing crashed?

Thank you very much for the info

 

[doubledog]

There was some fraction which have separated from solution, but did not seem that any separation of compounds occured - after drying, crashed material was still resinous,

To answer your previous question:
this ammonia IPA based resin was max 10% mescaline, so it contains mostly other compounds - salts, sugars, acids, phenolics, whatever.

 

[Loveall]

Sharing these results is extremely helpful doubledog. Since you already went through the HCl route, I'm now testing the sulfate route.

I added 250ml of 99% IPA to 75g of cactus powder. pH was at ~5.4 after mixing on my cheap plastic pH meter. After adding 25ml of 10% ammonia the pH barely reached 10. That was sealed and a couple hours later it was down to pH ~ 9.5 from reacting with the plant material I assume. Not a very high pH, but this is mostly an IPA medium thanks to your report (I assume you used 10% ammonia also) with the 95/5 IPA/ammonia ratio, I have hope that the Mescaline is in the IPA in FB form (I ended up with 90/10 IPA/ammonia).

Next, I'm going to boil the extract to remove as much excess ammonia as possible. After that I will titrate with sulfuric acid and see what happens.

Cheers.

 

[doubledog]

The pH seems rather low, I would go higher, but I did not measure it in my experiment.

For you that would mean too much water in your solution as you are using 10% solution.
More water, more other compounds (mostly sugars) extracted.
I would definitely let to macerate cactus in basic IPA for at least one day.

I used 18% ammonia.

 

[Loveall]

Ok, that means that we both ended up with ~1% ammonia solutions, but mine had more water (10% vs your ~5%). Was hoping for higher pH, but I didn't want to keep on adding ammonia for the same reason you mention (more gunk from extra water).

Do you remember the ratio cacti of powder to 1% ammonia solution you used?

Right now, I'm evaping the excess ammonia. pH is down to 8.5. I'm monitoring the ammonia release using pH paper on the fumes.

If I try this again I may try making IPA/ammonia mix and dry that over MgSO4 (MgSO4 is insoluble in ammonia)

 

[doubledog]

I used twice as more solution, and did two pulls.

I would say that pH 8.5 means mescaline is in salt form, not as FB.

Interesting, how do you measure pH on fumes?

Here is an interesting thread using basic alcohol:

An1cca's Mescaline Extraction "Peer-Review" Pictorial - Preparation - Welcome to the DMT-Nexus

 

[Loveall]

I used twice as more solution, and did two pulls.

I would say that pH 8.5 means mescaline is in salt form, not as FB.

Interesting, how do you measure pH on fumes?

Here is an interesting thread using basic alcohol:
An1cca's Mescaline Extraction "Peer-Review" Pictorial - Preparation - Welcome to the DMT-Nexus

I simply hold a pH paper strip over the fumes, if it turns blue still basic fumes. Right now, fumes look almost neutral (barely any color change). Before it was changing to a deep blue but I don't have a picture of that.

Thing about the pH, not sure exactly what it means in IPA. The dynamics are different than water. Different meter designs will give the same numbers in water, but in other solvents that is not guaranteed.

 

[Loveall]

After pulls and removing the ~1% Ammonia form the ~ 90% IPA using heat and monitoring the pH on the fumes until neutral, I added ~4x the volume in acetone to remove impurities (e.g. such as items that the 9% water pulled). The filtered solution was dried over MgSO4. This was titrated with sulfuric acid (going from basic to slightly acidic using pH paper).

After putting this in the freezer, a very fine white precipitate formed (could be anything, not necessarily mesc). I tired to collect it by filtering/decanting but it was nearly impossible and difficult to work with. The little bit I could decant reacted orange with Marquis though.

The process was interesting, but because of the practical difficulties found, I'm not going to put more effort in this path. Cheers.