First mescaline extraction a/b

[homobrassinolide]

So, I'm trying my first mescaline extraction.

I started with san pedro powder, methanol and 0.5 Molar HCl. I adjusted the pH to about 4 which is well below the pKa of a primary amine (~9.3). I heated this for 20 minutes. I then filtered the cactus material from the solvent. I did three pulls on it.

I then followed up with a little countercurrent distribution with xylene to remove most of the chlorophyll and what nots. I washed the acidic methanol solution three times with xylene.

I then adjusted the pH of the methanol solution to less than 11 (again pKa of primary amine is about 9.3) with 0.5 Molar NaOH. Obviously, everything then started precipitating out of the polar solution. I then tried to pull the alkaloid out with xylene and here is where things have not turned out according to plan...

Being that NaOH is a surfactant it made my methanol and xylene a whole lot more miscible to where I couldn't get any seperation. I then added naptha to get better seperation. I've been pulling on this solution with naptha a couple of times now. Correct me if I am wrong, but my thought is that the mescaline should be in the non-polar fraction after deprotonating the primary amine? It should be in the non-polar fraction because at a pH of 11 in a polar solution mescaline should have no charge and therefore be insoluble.

I still have a bunch of greenish-brown tar still in my seperatory jar. I have not concentrated/evaporated off the naptha solution yet. I was wondering how I was doing if someone could be kind enough to evaluate for me. Thanks.

[whatchamacallit]

Well the methanol should have been left out, and the pulls should have been done with toluene or xylene, as methanol is miscible with water.. Maybe evaporate everything, scrape up the mescaline and other crap that was pulled, then add basic water with a pH of about 10-11. Then do 3 pulls on it with xylene, combine them, then add acidic water (HCl and water) to salt it out. Evap the water and you should have mescaline HCl left..

[homobrassinolide]

Well the methanol should have been left out, and the pulls should have been done with toluene or xylene, as methanol is miscible with water..

I don't think you're following. I didn't try to pull from methanol with water. Both are polar, that certainly wouldn't work and I know that.

I've kept all of my fractions.

It seems that some of my earlier fractions from xylene/methanol are now settling out. Just takes a whole freaking day.

[bbd2]

naphtha is reputedly no good (read shit solvent) for mesc extraction
you need to use an aromatic solvent - xylene, toluene are common options
so goes the internet extractor lore

as for separating,
try making the polar fraction more polar - add basic water, nacl soln etc. something to discourage the xylene from being so miscible and friendly with the methanol

or you can wash everything with acidulated water - moving the mesc into it and going from there (this is what i would do)

or you can follow whatcha's advice - dry everything and restart

[bbd2]

Originally Posted by homobrassinolide

I've kept all of my fractions.

smart to keep all fractions <--- n00bs take notice

Originally Posted by homobrassinolide

It seems that some of my earlier fractions from xylene/methanol are now settling out. Just takes a whole freaking day.

or you can wait and seee what happens

[whatchamacallit]

I understand what you were saying but methanol is miscible with water and xylene, I believe, which will cause poor separation, if at all. SWIM would suggest evaporating the whole mix of solvents, then adding basic water, and pulling the freebased mescaline out with xylene. It can then be salted out. Trying to figure out where the mescaline is, in the mix of solvents (methanol, xylene, and water), will probably be a huge PITA, so it'd be much easier just to dry it all out, scrape up what's there, then adding basic water will convert the mescaline all to freebase, so it'll be pulled into the xylene. This will be the easiest way to get the crystals.

Methanol could have been used to extract the alkaloids and a bunch of other polar soluble plant crap, but then it would still need to be evaporated, then the leftover scrapings could be freebased, and extracted with xylene or toluene. Using methanol for pulling the mescaline out of a basic water solution may not work so well, because methanol is polar, and xylene is non-polar. Freebase is soluble in the non-polar solvent, not the polar solvent.

(Least polar)--petroleum ether
--------------cyclohexane
--------------toluene
--------------chloroform
--------------acetone
--------------ethanol
(Most polar)--methanol

[homobrassinolide]

Thanks. Sorry if I've been a jerk. Rough day. Anyway, yep gonna concentrate everything down, combine fractions, and use distilled water and xylene. Thanks yo.

[homobrassinolide]

It seems when I add water to my basic methanol/xylene fractions I get good seperation. Crystals are a comin'.

[kcmoxtractor]

Hell yeah, you better take pictures also!

[Fly on the Wall]

Instead of HCL you can use vinegar. Instead of xylene you can use limonene (orange oil). Instead of NaOH you can use CaOH. All food safe and non-toxic.

[kcmoxtractor]

Originally Posted by Fly on the Wall

Instead of HCL you can use vinegar. Instead of xylene you can use limonene (orange oil). Instead of NaOH you can use CaOH. All food safe and non-toxic.

I did the food safe tek, and it definitely works. He seems to have a good knowledge of chemistry, so let him do his thing. Take notes.

[homobrassinolide]

Hell yeah! What kind of a ride am I in for this weekend?

[homobrassinolide]

So after concentrating my non-polar naptha/xylene fractions down to about 750 mL, I've been pulling on it with acidified water. I dried one pull down already and I'm currently doing another. Gotta get me a new scale to give you a yield. I'm still gonna wash the crystals with acetone but they look pretty clean to me. They are a nice brownish-white salt.

[ktownhustla]

wouldnt chorlphyll be soluble in both xylene and meoh