Dry solvent confusion?

[dumbstruck]

In the lye water and cactus -> xylene pulls -> hcl water -> evaporate method of extraction the xylene isn't dried. But both the mescaline freebase and the salt should be "moderately soluble" in water. Is it because we are pulling the salted mescaline out into a layer of water that drying the xylene is unnecessary? Or is there loss in that step? I know ~3 hcl water pulls are usually done to each xylene pull, so is that to minimize the loss from the water in the xylene? That makes sense I suppose, but seems like an awful lot of extra work, especially having to pull the water off the bottom and all that.

I always assumed we don't salt it directly out of the xylene to avoid as much xylene contamination as possible. I was hoping to use MEK to avoid this issue. It is not so nasty and the freebase should be highly soluble while the hcl salt completely insoluble. Also considering the fast evaporation then salting out directly should be no particular problem.

Here is my current plan. Take 4 parts cactus and add 1 part calcium hydroxide, add small amount of water and mix for a few minutes, dry completely in an oven on low heat (should be stable even ~200 F, right?), crush back into powder, then pull with MEK.

So for this next step should I pull with hcl water (or vinegar for that matter) or should I try to salt the alkaloids out? The salting should be more efficient if the MEK is dry right? How long after drying do I have until the MEK is back to 5-8% water or whatever it is when stable? So how long would I be able to use it for pulls and then salting before I get significant loss?

 

[narmz]

The reason you don't dry the xylene is because it is an aromatic hydrocarbon, meaning it cannot/will not contain any water and is not miscible with water in any amount. The problem with using mek is that it is not aromatic and can absorb water. So trying to salt using hcl water while using mek will result in most of the water mixing with the mek and you will be unable to retrieve your product without completely evaporating it.

There is no reason not to salt directly out of xylene if you can, because the product obtained in this way is very clean, and if you dry the product thoroughly there will be no more contamination than with any other method.

If you plan on using MEK, I would think that salting the alkaloids out directly would be the best method to go with if possible. Always make sure your solvents are dry with anhydrous magnesium sulfate or calcium chloride, this will ensure no product is lost.

 

[dumbstruck]

Very interesting. If I mixed a few drops of 30% HCL solution into 50 ml of acetone, would the HCL migrate from the water to the acetone in any amount? So could I then use that to salt out from the MEK or xylene (as acetone is conveniently miscible with water and xylene)?. There would only be 1/10th of a ml of water added from the HCL solution. With the MEK I was thinking I could use saturated MEK to salt it out, but again am confused with how exactly HCL gas dissolved in water will act mixed with another solvent.

I could also easily use any acid that happens to be soluble in xylene or MEK, but heavens if I know what they are. I believe I'm still going to try the dried MEK over the xylene, but that is only assuming I have at least 5-10 minutes before any appreciable amount of water gets sucked back in. Any input on this time frame would be greatly appreciated. If not I am very happy skipping the extra hours and hours and hours it takes to freeze off bottom water layers repeatedly and just figuring out how to salt from xylene.

Thank you, narmz, that made everything make sense again.

 

[dg]

and just figuring out how to salt from xylene.

Thank you, narmz, that made everything make sense again.

if you want to filter salts directly from the extraction solvent, you can.
gassing is very effective, but the crystals formed will have inclusions of the solvent, that standard acetone washes will not remove- not w/o re crystallization will this yield clean material.

best to use water to get the alkaloids from the xylene/toluene, then force the alkaloids out out of the much cleaner secondary solvent(crash or crystallize)
or easier(but takes longer), dry the water to a tan/brown powder and re-x with mek or acetone

 

[narmz]

Very interesting. If I mixed a few drops of 30% HCL solution into 50 ml of acetone, would the HCL migrate from the water to the acetone in any amount? So could I then use that to salt out from the MEK or xylene (as acetone is conveniently miscible with water and xylene)?. There would only be 1/10th of a ml of water added from the HCL solution. With the MEK I was thinking I could use saturated MEK to salt it out, but again am confused with how exactly HCL gas dissolved in water will act mixed with another solvent.

Yes, you can do this, though SWIM has never tested with mek. You can definitely do it with xylene and acetone. Basically you add some HCL solution to the acetone, and then dry the acetone using anhydrous magnesium sulfate or any other dessicant to remove the water. There can't be any water present. Then salt it directly out.

Even easier, is to salt the alkaloids out using Fumaric acid saturated Isopropyl alcohol. Mescaline fumarate will fall straight out, and will continue to fall out of the solvent for days. SWIM just performed this on some 300ml of limonene - 200mg (after being cleaned) fell out the first day, a couple hundred more fell out the next day, left it for a couple days, and a good 500mg (after being cleaned) fell out again. Clean the product with dry IPA or Acetone or MEK. SWIM has tested all three and they all work but SWIM prefers IPA because it evaps quickly and doesn't stink as much.

The potency is very close to HCL, SWIM thinks it is a 2 to 1 salt, so it should be about 91% as potent as hcl, if i am wrong about it binding to 2 freebase molecules then it is about 75% as potent which ain't bad either compared to some other salts.

SWIM and his girlfriend tested out 400mg each of the substance and found it to be on par with a 360mg mesc hcl experience they had in the past. Seemed to almost last longer than the hcl salt.

Cleaning and redissolving in water and slowly evapping on glass gives crystal structure similar in appearance to mesc hcl.
SWIM suspects the tartaric acid salt of mescaline would work nearly identically but be slightly less potent than the fumarate salt. SWIM was amazed at how much mescaline fell out in the end, so even if you think it's all clear and you decant it, save your solvent in a clean jar, more will most likely fall out in the days following.