Greetings! Im about to undergo an extraction using Endlessness ethanol tek https://www.dmt-nexus.me...aspx?g=posts&t=30501 and something came to my mind. This tek leaves alot of sodium carb in the final product when ethanol isnt anhydrous, and some people seems to not being extracting as much dmt as they could from this tek, although this doesnt seem to be consensus. I was considering drying my 95% grain ethanol with some 2g sodium chloride for each 100ml as it is very soluble in water and almost insoluble in ethanol. Also, Im guessing this would increase the ionic strenght of the polar layer of the mix mhrb-sodium carb paste/sodium chloride ethanol, forcing the sodium carbonate to stay out of the ethanol while all dmt and other alkaloids soluble in nps stuck to it ala Cyb/CTM Max Ion Tek. Then I would evaporate the ethanol, and recrystallize the remaining goo in heptane via freeze-preciptation. Is this proccess possible? Also, if I were to clean the resulting goo with an acid step before recrystallization, would citric acid be a suitable choice? If yes, in which ratio to water? Vinegar smell sucks! Thanks in advance!
|
|
|
I'm on my way out the door and will adress your other questions on my brake, until then this may be useful: In regards to preparation of anhydrous EtOH: anhydrous EtOH preperation video-eg
|
|
|
Nice video! Didnt know about molecular sieves.
Something I was thinking after watching it, I could substitute sodium chloride for magnesium sulfate perhaps? Ive seem a post from cyb where he states magnesium sulfate can increase the ionic strengh of the aqueous layer by 4x more than sodium chloride. I know the liquid phase of the system will be homogeneous as ethanol is both polar and non-polar, but with the ionic strenght of the solution increased, it would behave much more like a NPS, no? I feel safe to assume that as magnesium sulfate is hardly soluble in ethanol. Just gotta be sure there will be enough liquid for the reaction to occur completely.
Is that correct?
PS: for someone wondering why I dont want to simply re-x with heptane rightly after basification/salt addition step, its because I want to keep the goo separate for some change later, but cleansening it a bit from excessive residues that might be in it.
|
|
|
You cannot dry ethanol using sodium chloride. Sodium chloride does not form hydrates, so it cannot absorb water into its crystal lattice like eg. anhydrous magnesium sulfate can. When mixing salty water and ethanol, the salt will crash out of the water and ethanol mixture. You can actually push water out of ethanol to a degree using potassium carbonate, but it will not go beyond 95%, which is what you state that you already have.
The endlessness tek is not comparable to an A/B, STB or hybrid A/B-STB tek like cyb's. The latter all use phase separation between a polar and a non-polar solvent. Endlessness' tek uses no phase separations and no non-polar solvents. It's a different method altogether.
I doubt if using anhydrous ethanol is an improvement, because there is water involved in most steps anyway. Even if reducing water was useful, you'd probably better invest efforts into making the sodium carbonate (commonly sold as a decahydrate) anhydrous. But then water is added to the dried soda afterwards anyway.
|
|
|
You offered some good insight pitubo, thanks alot!
Here's what Im currently considering doing:
1 - Mix mhrb + excess sodium carbonate + saturated magnesium sulfate water (to the point of the water be still saturated even after the ethanol pulls) enough for it to become pasty
2 - Let it totally dry, then pull 3x with ethanol that would be anhydrous when in contact with excess MgSO4 still present, then filter and evap. Some shaking during the pulls perhaps?
3 - Wash the resultant goo in filtered tap water to remove any polar residues
OR
Go straight to re-x with heptane/freeze-precipitation
4 - Save the goo for changa and weight the whitey pure dmt yield
I want to do this as simple as possible as I messed things up trting q21's A/B tek. Im wondering though if pulling with ethanol is a redundant step as I have heptane available, or if it will really aid in obtaining a purer goo. Gotta read some STB teks again.
|
|
|
even anhydrous MgSO4 is not always enough to dry ethanol beyond its azeotrope, it really likes to hold onto water. But even still, it shouldn't a be a problem with your method, since you also plan to re-x. Keep in mind, the ethanol is polar enough, it will still pull a lot of coloured crap that heptane wouldn't. I don't think a water wash of the goo will do a good enough job, I think you should go right for the heptane re-x. Or, better yet you could combine the two, dissolve the resulting goo you get in acidic solution, do a mini-AB and extract with the heptane then crystallize. This is essentially what I do in most cases extracting any alkaloid, use the inital ethanol extraction to reduce the overall amount of material, then clean it up with an acid base, its much easier to work with a few grams of material than a few hundred grams. Expect nothing, Receive everything. "Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). " He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita "The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
|
|
|
Thats neat, thanks alot Mindlusion!
Do you find citric acid to be suitable for further cleansening the goo? I dont like vinegar but might consider it otherwise as it will require way smaller amount of it.
|
|
|
Citric acid will work, although some prefer fumaric acid as it is easier to crystallise the fumarate. Quote:1 - Mix mhrb + excess sodium carbonate + saturated magnesium sulfate water (to the point of the water be still saturated even after the ethanol pulls) enough for it to become pasty sodium carbonate + magnesium sulfate will produce (basic) magnesium carbonate as an insoluble precipitate, plus sodium sulfate which is of little use for drying ethanol but will still increase the ionic strength of the paste somewhat. Equation: Na 2CO 3 + MgSO 4 = Na 2SO 4 + MgCO 3 (+ Mg(OH) 2) Quote:2 - Let it totally dry, then pull 3x with ethanol that would be anhydrous when in contact with excess MgSO4 still present, then filter and evap. Some shaking during the pulls perhaps? You'd have to bake the paste to to make anhydrous magnesium sulfate, which for one thing would vaporise much of the DMT present and as stated above there wouldn't be any magnesium sulfate left anyhow. Better off using a dessicating jar with a suitable drying agent if you want to experiment with anhydrous sodium carbonate paste, etc. “There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work." ― Jacques Bergier, quoting Fulcanelli
|
|
|
This anhydrous thing is too complicated for the presumed benefits from it. Perhaps I should just do a mini A/B on the goo then re-x and forget about the jungle spice... NEVAH!! Gotta try to figure a way to have my jungle...
|