Cactus extraction - bad xylene used.

[sswim]

Hi everyone,

I came here to tell the story of someone stupid who isn't me who didn't think enough about what exactly is in the tin bottle as it was the only thing available.

So here it goes. SSWIM used around 200g of fresh cactus (panch.) and blended it with a bit of water. Then cooked it well for an hour with more water a few grams of citric acid. SSWIM did this 3 times and composted the remains. Cooked down the water a little bit.

SSWIM then did some "bad xylene" fat removal and then used dissolved NaHO until PH was 10 and 3 Water pulls and used a bit of citric acid on the water, ph changed soon to mildly acid.

Now SSWIM tried to reduce the water but was soon left with a brown thick paste that smelled a bit like vinegar.

SSWIM then proceeded to read up and dissolved the paste in a bit of water and a few ml of 35% HCl Acid. He tried to freeze precipitate but nothing came out of it. Froze solid without crystal formation.

After SSWIM searched the interwebs for the datasheet of the xylene he found that it contains a good bunch of acetone and other stuff.

So now SSWIM takes the xylene and mixes it with excess water and a good bit of NaCl, shakes well and takes only the top layer. SSWIM then takes the hopefully better xylene and does a clean / freebase with NaOH / pull with xylene / HCl-Acid salting process on the remaining liquid and tried again to freeze precipitate but again froze solid.

My guess is that SSWIM has nothing left in the water, most interesting stuff is most likely gone with the acetone a long time ago and anything left after drying is NaCl.

 

[sswim]

To clarify, SSWIM used the "clean" xylene to do a whole round of extraction on the goo watery mix.
SSWIM has now added around 20 drops of H2SO4 3.5% to convert to mescaline sulfate, mixed thoroughly and put the water back into the fridge.

And I should have asked a question or two.
Do you think there is anything left? Do you think SSWIM was able to clean the xylene good enough?

 

[GratefulDad]

First off, maybe you mean xylene? I don't know of any solvent called tylene. Also, you can't freeze precipitate mescaline from xylene or toluene, only DMT freeze precips from naphtha, or some of the chemicals that make up naphtha, such as heptane.

First you can boil your cactus in acidic water, separate, and repeat with fresh water, then cook it all down to a smaller amount of liquid. You could then defat with a non-polar solvent, but I find it completely unnecessary, as a defat doesn't really do anything IME, to make the final product cleaner. After you remove he xylene layer (if you did defat), you discard it properly, then make the acidic cactus water basic with something like sodium hydroxide, aka lye, aka NaOH. OR, you can just mix your cactus powder into lye water, without all the cooking in acidic water and filtering steps.

Next, making your cactus water more basic would likely pull out more mescaline (in other words, convert it from the water soluble citrate salt, or whatever acid you used, to a freebase), as well, as the pH of ten is very close to the pKa of mescaline, so it might not have all converted to a freebase (most probaby not!) at only a pH of 10. 12-14 would be better to make sure you get all the mescaline converted to a freebase and into the non-polar solvent (xylene), that you mix together very well with the basic cactus juice and let sit until the layers separate.

Then after separating the xylene from the basic cactus water, you add your acid (or acidic water) to your solvent (xylene) containing the freebase, to convert your mescaline freebase back into a salt. Doing three to four solvent (xylene) pulls on sufficiently basic (pH13+) cactus water should pull out all your mescaline. You can save all the portions of xylene and combine them, or just do one pull at a time, salt the mescaline out of the xylene, then repeat until you no longer get out any more mescaline.

If you use vinegar (or acetic acid), you'll get mescaline acetate, which is usually a paste or waxy solid that is hygroscopic, but can turn brittle with time, which means it will pull moisture from the air and be very hard to completely dry. It will give you a paste or waxy substance containing your alkaloids as acetates.

If you use hydrochloric acid, you'll get mescaline hydrochloride (HCl), it will dry easier, but if you use too much, it will come out from tan to dark brown. This is fine to use as is (when it's completely dried), but it can be cleaned up by recrystallizing, or in the future, try 4 drops of hydrochloric acid to 100 ml of distilled water, as this always seems to make my HCl crystals white, or sometimes just off white (but still much cleaner).

When using sulfuric acid, you'll get mescaline sulfate (pretty needle-like crystals), but it's best to gas the acid through the solvent so you don't overdo the sulfuric acid (or do precise calculations), because it does not evaporate when completely dry like hydrochloric, and can leave your mescaline sulfate with excess sulfuric acid in it.

 

[sswim]

Yes, thanks for the correction - its indeed xylene. Fixed in the post.

SSWIM hasn't used vinegar but it smelled like it contained some after reducing.

Now the water is clean and all that is left. Not sure what is still inside.