Need help ironing out a new lab glass dependent tek

[Afrikaaner]

So this is my basic idea:

* Pack a Soxhlet extractor or similar with MHRB, and do an extraction with muriatic acid for several hours.
* basify solution to deprotonate the DMT and make it soluble in non polar solvents.
* evaporate all (most?) water, being careful to not overheat the resulting powder or goop or whatever it turns out to be.
* repack the Soxhlet extractor with the evaporated extract, and this time extract with your choice of non polar solvent.

It's not particularly different from a regular A/B extraction, just contained in labware. Another idea I was tossing around was this:

* soak, then freeze and thaw the MHRB several times to lyse the cell walls
* skip the acid and base stages and do two Soxhlet style extractions, one with DI water (to get any already protonated DMT and DMT oxide naturally found in the cells), then again with a non polar solvent (to get any freebase, etc DMT)
* evaporate the non-polar solvent, and dissolve the recovered solids in the water (as best as possible)
* convert DMT oxide to DMT using 69Ron's DMT n-oxide to freebase DMT tek (I need to confirm this is viable)


I'm particularly curious about the second option, as it seems like it would be much easier than my current STB using milk jugs tek. I was also curious if you could replace the polar and non polar solvents with a single semi-polar solvent like xylene.

All comments are welcome, I'm just sorting this out in my mind before I start experimenting, and any experience with similar topics is VERY appreciated. Cheers!

 

[benzyme]

well, these are all ideas that have been thrown around in several threads; make some quality posts and you'll get access to them. acid in the soxhlet won't work as you'd expect, because the water condensing over the plant material would have neutral pH (aq. HCl is azeotropic)

xylene is only slightly polar about the aromatic ring structure, as "resonance" occurs in its
pi-bonds. it's an overall non polar molecule, because there is no dipole moment.
that being said, single solvent extractions do nothing to isolate alkaloids from other biomolecules.

 

[a1pha]

; make some quality posts and you'll get access to them.

Level 2 activated. Welcome.

 

[Afrikaaner]

benzyme, thanks for the post! my understanding of azeotropes is a little different (though possibly entirely wrong). My understanding was that being an azeotrope, that at a certain point (around 22% I think for HCl), the two are no longer separable by distillation, meaning that the water vapor in the setup and the condensed water vapor on the condenser/in the soxhlet would all be of the same acidity. Is my general understanding incorrect?

 

[benzyme]

you're correct


alcohol in the mix improves the distillation efficiency.
here's a good thread on relevant experiments

 

[Afrikaaner]

excellent information, do you have any futher details about forming azeotropes? I can't seem to find anything good about them...

 

[pitubo]

As I understand it (I am not a chemist) indole, and therefore tryptamines, are somewhat sensitive to strongly acidic conditions. Maybe refluxing in HCl is not the best thing to do here.

Perhaps using dilute acetic acid instead is a better option. Also, since water and acetic have very similar boiling points, the concentration of acid flowing through the soxhlet would be more or less the same as in the boiling flask.

 

[downwardsfromzero]

you're correct


alcohol in the mix improves the distillation efficiency.
here's a good thread on relevant experiments

It's a good link; I was about to suggest using a blend with calcium hydroxide, like this post, albeit using a different non-polar solvent or IPA.