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The Minimalist’s Mescaline Microwave Assisted Drytek

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For completeness, I went back to the titrated acetone from the previous post. It was evaped to a gunky syrup where the excess sulfuric acid concentrated. Based with NaOH/water and pulled with Limonene. FASI showed some clouding, but it was minimal (maybe 30mg, I'll measure it and report back). I think this indicates that > 97% of available mescaline was precipitated from the acetone solution during titration.

Well, I stand corrected. Measured the mescaline candidate pulled from the Limonene and got 180mg. This re presents ~0.2% of the starting material and 6% of the candidate product that crashed from the acetone (original process potentially pulled 94%, not >97%).

Based on this, it could be worth drying the paste more before doing the acetone pulls to see if what doesn't crash from the acetone/water can be reduced. For example, if the cacti powder where only 0.5% mescaline (and the rest of the yield is other stuff), we wouldn't want 0.2% to not crash from the acetone due to (supposedly) the presence of water.

Note: For me, in practice, it was a lot easier to work with the acetone/sulfuric acid system than the Limonene/FASI. Easier to collect from the solvent after crashing (fine particulates escape the filter with FASI salts and not with sulfates), easier to scrape up after drying from water (FASI salts required elbow grease) and easier to wash (FASI salts didn't stay down when decanting).
Thanks DWFZ and Wolf. Benz analysis is back, and unfortunately despite getting the Marquis reaction orange color, it turns out there is no mescaline or alkaloids in the process using this "shortcut".

So it doesn't work :(

Since the known liomeme/FASI worked on what didn't crash from the titrated water/acetone pull I think we can say that mescaline sulfate does not crash out even in water/acetone that was in the freezer. I guess there was probably just too much water, since in dg's protocol it does work when the water is concentrated.

For this to work, full chemical drying like ACY suggested seems necessary. Need to make sure to keep things basic when using the slightly acidic MgSO4.

At least I believe I learned something 😅

Back to the drawing board. Cheers.
I've been working on this approach (but skipping the acid part) and can't get it to work well/reliably with acetone. Mainly, crashing from acetone has been hard for me (tried sulfuric, HCl, and various organic acids including fumaric, malic, and citric). This includes both air-dry and chemical dry with MgSO4 of the basic cacti paste. It also includes wet paste with 50% NaOH to keep the acetone dry, and drying the acetone after the pull with MgSO4 and/or NaOH. After poor salting results (only got some small amounts of product here and there), acetone evap and A/B recovered the bulk of the product from the acetone. I understand it is possible to get salts from acetone (e.g., dg's sulfuric Tek from water/acetone), but that is from a concentrated and clean starting point. As doubledog has pointed out it is not so easy when closer to the plant and on dilute conditions.

If I use limonene indead of acetone, then crashing with FASI works well and effortlessly. Also, don't need to dry the cacti paste completely. Instead, I find it more practical to have a slightly wet paste, making limomene and water/cacti separation trivial (just pour off). I let the limomene settle for over MgSO4 until it becomes clear (after pulling it can be cloudy), and decant that into a salting jar for FASI salting.

This is nothing new. It is just 69ron's limomene Tek with ACY's microwave assistance added (which makes it easy to get a good paste consistency), and FASI salting (mentioned by for example narmz). It all works great together 🙂

The process I like is (again, these are all other people's ideas, not mine),

- Microwave cacti powder/water/Ca(OH)2 to a smooth paste. Add NaCl (optional), pull with limonene, and rest over over MgSO4 until clear. Decant clear limonene and salt with FASI slowly. Recover salts and wash with dry acetone to remove limonene. For a more crystalline product dissolve salts in hot water and allow to evaporate slowly. At this time product tends to be a little pink/salmon, more acetone washes can whiten it up if desired.

If anyone is interested I can write this up with more details/pictures. There is no layer separation, no possibility of emulsions, and no cacti filtering. Cooking is limoter to a few minutes in the microwave. Yields seem good to me. The limonene can be washed with water and reused.

I think the limomene/FASI salting should be added to the wiki as a mescaline Tek too (I can't find it there). Perhaps as an update to 69ron's limonene tek. If starting with fresh cacti, I imagine that simply blending with Ca(OH)2 and microwaving to get to the paste would work.

Disclaimer: These are just my personal preferences and observations at the moment. I'm not claiming this process is better than others which also work well. Again, none of these ideas are mine, but I wanted to summarize/conclude several work threads on what I have personally settled on as practical and easy.

I am really interested in your approach with wet basic paste. If you can elaborate more on that, I would appreciate.
When I tried something similar, I lost a lot of NPS (I use toluene or xylene) trapped into cactus solids. If there is an option to avoid long cooking and reducing of cactus soup, that would be perfect, as remaining steps of extraction, once freebase is in the nonpolar, are quite easy.
I'd also appreciate more info on this process. Not been getting good yields with 69ron type drytek and dont have time for long boils atm.
Sure thing, next time I will take pictures and have more details. For now, here are my observations:

- I think the key is for the paste to not be too wet and to also stir slowly (think of boiling pasta, not whipping up egg whites)
- I personally found 69ron's Tek, 12:4:1 water:cactus:Ca(0H)2, to be a little too wet for limonene mixing/separation
- However, 69ron's ratio is good for initial mixing. Starting at that ratio, I add the water to the jar, then add the cacti powder on top slowly while mixing it in (to avoid dry clumps - think of making mac n cheese), and finally Ca(OH)2. Mix until smooth.
- To get the right consistency, Microwave in bursts (~4 minutes to heat it up, then 1-2 minutes with stirring in between). Microwaving the paste can be a little stinky. Keep track of the water weight so ratio gets to ~8:4:1 or even lower (I'll post a more exact ratio next time I do this). In my microwave (1700W) 1 minute removes ~10g of water weight. The microwave definetly also does something to the consistency of the paste (more workable).
- Based on the water weight left, I add ~25% salt to the paste. This is just hoping to increase the partition coefficient and to lower limonene absorption (haven't done a split experiment to verify).
- I did notice some limonene absorption in the first pull, but didn't seem like a lot (I'll keep track of the weight next time). Also, 2nd pull and beyond had no noticable new limonene absorption.

- Debugging: I've had the limo significantly soaked up into a more runny paste that wasn't microwaved. It was on my first try and I had too much water and stirred to fast, effectively whipping the limo into the paste like a soufflé. I added MgSO4 and some dry cacti powder and thankfully the paste clumped up releasing a lot of the limo (this brought a smile to my face). It was not a full release, since by waiting for a day or so, some limo had "sweat" out of the paste.

PS: A note on the microwave stinkyness. It's not too bad, but sensitivities vary. When mixing in the Ca(OH)2 there is a faint ammonia smell from the lime/plant-stuff reaction. I imagine if the jar is left alone uncovered for a day or so it will mostly dissipate. Microwaving after that may be more pleasant, but I'm just guessing.
In a new test to try to maximize partition, I completely dried the Cati/lime paste with the microwave and MgSO4. This was ground and pulled with limonene. It didn't work: some mescaline came through but it was very minimal. Interestingly, adding water back to the paste (1.5x the mass of cacti) and doing a limonene pull again reversed the issue and worked great.

For some reason the presence of water is important to get mescaline FB to move from the cacti into the solvent in this example. Issues with complete dryness were reversible as yield was fine after rehydration. Something happened to mescaline FB when I dried it that made it not go into limonene. I don't know what that that thing is, but that is what I got.

After all these tests, I'm finding that ron69's limonene tek works well, but I personally like modifying the alkaline paste by reducing the water:cacti from 3:1 to 1.5:1 in the microwave (using a scale to track water weight) and then adding ~25% of the remaining water weight as salt. For me, this gives a more workable paste that gets pulled relatively well with limonene. I now prefer to salt the limonene with sulfuric water, titrating to neutral pH, and after reducing the water adding acetone to get the sulfate crystals as described in dg's thread.

Note: FASI has not always been consistent for me since my last update: sometimes (not always) the precipitate is too fine to catch easily in the filter, which is a pain. I no longer go this route
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