Extraction Method Clarity

[proefbuis]

I'm just trying to comprehend most of what's going on in the basic sequences of an A/B extraction. I have read every tek, I believe, and often find conflicting opinions. I have an idea of what I think would be the most prudent tek, in terms of apparatus availability. Please correct any errors or misconceptions in my method.

Chemical Apparatus:
vinegar/acetic acid (CH3CO2-)
naptha (hydrocarbons)
lye (NaOH)
water (H2O)

Method:

-Add the powdered bark species of choice to a water and acetic acid solution with a pH between 2-4. Heat the solution with added material.
*this should form DMT acetate salt if not already in this form? *
Remove and keep in sealed jar until cool.

-Basify the solution with the introduction of sodium hydroxide and bring the pH to approximately 7.5.
*i've read teks that instruct a pH of >~9.5 and one saying to reach the highest you can achieve. Would this work, as the pKa of DMT freebase is 8.68 according to the Merck index? Is this intended because it should dissociate the compound? *
*this should form DMT freebase? *

-Extract the DMT with a non-polar solvent, in this case Naptha, by adding it to the basified solution. Do a number of pulls and pool them.

-Freeze precipitate.

This is one solution being changed throughout until the DMT is pulled.

 

[diox8tony]

...

 

[proefbuis]

Although, how does the acid remove the unwanted compounds, in my idea the solution is the same when NaOH is introduced, ie. no further extractions at this stage. (what happens to them)?

With that, in the 'DMT Extraction Overview' on this site the author posts;

"(Optional) First Defatting Opportunity (Acid/Base Extraction Only)
If you made an acidic extract of the DMT salt, you can now take the opportunity to remove unwanted plant fats and impurities by extracting your acidic solution with a couple volumes of nonpolar solvent and the solvent discarded. Naphtha, toluene, or xylene are all acceptable for this step."

*The author implies that the DMT acetate is non-polar? *
Also, I don't really understand the instruction. The DMT acetate is extracted into the solvent, then what, obviously something is missing before 'discard the solvent'?

Does it mean;

*Convert to _acetate,
*Extract (polar/non-polar solvent..I'm not sure now), *has naphtha got characteristics of both a polar and non-polar solvent? *
*Freeze precip.,
*Convert to Freebase,
*Extract (again, polar/non-polar solvent..I'm not sure now)
*Freeze precip.

 

[Mr. K]

diox8tony is very close in their explanation, but when the dmt is in the acidic form during the acid bath it doesn't actually remove the fats from the solution. The acid wash serves to break down the root allowing more dmt acetate to be available for the later extraction.

proefbuis,
The quote you gave of the author is correct. I'll try and explain. When the dmt is in the acidic extract the dmt is not soluble in the non-polar solvent. The non-polar solvent is added after the acid bath to remove plant fats and oils which tend to leave the final product more yellow and more of a sticky consistency rather than crystals. The non-polar solvent can be thrown away because there is no dmt in the solution. After the defatting procedure, the acidic extract is then basified converting the dmt acetate to dmt freebase. After the dmt is convertated to freebase is it now soluble in a non-polar solvent.

So, a general step by step of a/b
*acid bath (convert to acetate)
*defat (pulls out plant fats and oils)
*basify (converts dmt acetate to dmt freebase
*pull with non-polar solvent
*freeze precip

also with the ph, the higher the ph the better, most teks I've seen call for a ph of at least 12. It can't hurt anything going that high, it just makes sure you get all the goodies out of it.

Good luck and cheers!

 

[gibran2]

When using powdered bark, the acid step is done simply to ensure that all of the DMT is in a water-soluble form that won’t evaporate or otherwise break down when heat is applied. Generally, acid pulls are collected and boiled vigorously to reduce volume to a manageable amount. If a basic solution containing freebase DMT were boiled, much of the DMT would evaporate and thus be lost.

 

[proefbuis]

Fantastic, I understand that perfectly. Just out of interest, would you be able to show formulae of the extraction pathway:

form of DMT in bark(?) + acetic acid(CH3CHOOH)-> DMT acetate(?)
DMT acetate(?) + sodium hydroxide(NaOH)-> N,N DMT(C12H16N2)

Much appreciated.

 

[gibran2]

Fantastic, I understand that perfectly. Just out of interest, would you be able to show formulae of the extraction pathway:

form of DMT in bark(?) + acetic acid(CH3CHOOH)-> DMT acetate(?)
DMT acetate(?) + sodium hydroxide(NaOH)-> N,N DMT(C12H16N2)

Much appreciated.

I'm not a chemist, but I think it goes something like this:

DMT-tannate + acetic acid --> DMT-acetate

DMT-acetate + NaOH --> sodium acetate + DMT freebase