Theoretical extraction without naphtha and fumaric acid???

[Murdoc]

Hello this is my first post here on Nexus so hello to all of you nexians!!


i have a bit of struggle with getting pure naphtha all of them pulls only oily jungle spice....so it must contain some xylene or toluene...

So i came up with my own tek that do not need naphtha or fumaric acid.
Remember this is just theoretical and i havent yet tried it but i will in up comming days.

Experimental

V 1

---Portuguese Armada's J TEK---

-Supplies
1.MHRR or ACRB
2.NaOH
3.Toluene or xylene(xylol)
4.Acetone
5.Citric acid
6.Lime Ca(OH)2


1.Measure out 50g of MHRB OR ACRB and grind it up in fine powder.

2.Take 50g of NaOH and slowly add it to 650-750ml of slightly cold water

3.Add grinded bark to sodium hydroxide solution

4.Shake shake shake and let it sit for a while

5.Add toluene 75ml (???) mix it around same as naphtha and wait for layer separation...
maybe warm water bath will help to pull more alkaloids....separate solvent layer and keep it

6.Repeat step 5 three more times

7.So now you have to add citric acid to distilled watter... not too much not too less...Just small amount of water

8.Add acid solution to toluene and mix it around and wait for reaction to end and layers to separate...I know i know citric acid is not good cuz it makes dmt goooe oil rather than crystals same as acetic acid. But in theory now all alkaloid citrate salts should be dissolved in water layer.

9.Separate water layer (toluene could be reused)

8.Now add Ca(OH)2 to water that was separated from toluene...it should be pasty like consistency...now citrate salts are converted in freebase.....Paste should be fully dried out of water

9.Now crush up paste and mix it in acetone freebase should dissolve in acetone but calcium salts should not..

10.Evaporate acetone and collect your freebase alkaloids....




This is still just theoretical i havent tried it yet as i stated before

Maybe even someone have tried this and this isnt anything new


the question is if i pull with toluene and convert it to citrate salts will i still end up with jungle spice because off all pulled alkaloids are salted and then freebased with lime???



Thanks Murdoc

 

[downwardsfromzero]

Yes those standard steps should work, assuming your plant material is any good.

It's a matter of combining various steps that work using the reagents and solvents available - so you've come up with one of a number of permutations.

As far as 'Jungle Spice' goes, I can't really comment although a thread describing analysis of such found it to be about 99% DMT anyhow.

 

[downwardsfromzero]

One person has reported success with recrystallising citrates. It may be a stoichiometry thing, citric acid being tribasic and all that. Can't find the thread though. I seem to recall there being some question about the acid/base ratio of the crystalline product, at the very least.

 

[Murdoc]

yeah my best bet would be fumaric acid but while i wait for it to arrive i can try this method...fumaric acid is nowhere here to be found so i got to use internet for that... also stb is problem because naphtha here is crappy brands with a lot of other additives to it....still got half kg of bark to work with. Its easier for folks in usa to get all supplies.

I just added toluene to bark and sodium hydroxide mixture....i will separate them tomorrow and continue according to my theoretical tek adjusting and tweaking it along the way..

 

[blue.magic]

It may be a stoichiometry thing, citric acid being tribasic and all that.

Yeah - if the target amount of alkaloids can be guessed, one could calculate the amount of acid needed.

Maybe it's like with mescaline - carefully titrate (ideally with monoprotic acid, e.g. acetic, so no jumps in pH) until the water layer gets very slightly acidic (sign that all the alkaloids have been converted and pulled over to the aqueous layer).

I guess the pH need to be checked carefully as the excess acid would cause pulling unwanted substances (at least this happened to me with mescaline).

 

[downwardsfromzero]

There's a similar knack towards separation of alkaloids from a mixture to be seen with the ongoing harmala alkaloid separation efforts over in the exceptionally instructive ...finetuning of the VDS-protocols thread. There's the application of carefully controlled pH levels to facilitate separation of some quite similar alkaloids. Whether that method could be applied to a mixture of cactus alkaloids depends to a large extent on the relative pK values of the individual alkaloids. Not to mention a component of enthalpies of crystallization. You can't guarantee that the mescaline will be pulled first without some research, both literature and practical.

Then there's the exploitation of differential solubility parameters, hence the use of acetone and MEK washes.
And before you know it, you're contemplating preparative chromatography :lol:

The thing about citric acid (besides its hydroxy group...) is that it can combine with 3, 2 or 1 equivalents of univalent base - such as a protonated monoamine - which may make the pH curve unfavourable for obtaining sharp separations.