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Acids/Base Acetone Theoretical TEK

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delta-9

delta-9

Rising Star
Hi there everyone, I have not tried this method yet, and I want to know do you think this would work?

Reasons for wanting to take this approach:
-Where I live naphtha is very expensive, acetone is cheap.
-DMT is soluble in acetone and does not require heating, safer than heating naptha
-Also I dont want to work with xylene because it is nasty.

The main principle I will be using is that freebase DMT is highly soluble in acetone, but DMT fumarate is insoluble in acetone

This is essentially a modified version of Q21Q21's @fluffy white funfest' A/B tek, however instead of naptha I plan to use acetone as the non-polar solvent.

Step 1- Acidification with Vinegar

Step 2- Basification with Calcium hydroxide, (lime)

-Now here is where is where the difference comes-

Step 3- Non polar wash with acetone (any advice on how much?). Allow acetone to take up the freebase DMT. Pour off into a separate vessel, this will be called the 'pull'

Step 4- Add fumaric acid to the pull until acetone is converted to FASA

Step 5- Wait for DMT fumarate to crash out of solution and crystallise (how long would this take??)

Step 6- Filter contents to separate the DMT fumarate solids, with filter paper and funnel

Step 7- Wash with some cold acetone to remove excess fumaric acid

Step 8- Place DMT fumarate on foil to dry- if fumarate salt is the desired product finish here. Or, If freebase is required go to step 10

Step 9- Dissolve DMT fumarate in minimal amount of water, add Calcium hydroxide to convert to freebase. Allow water to evap, then dissolve freebase in acetone and pass through filter paper, keep the acetone. Then evap the acetone for near pure DMT freebase, recrystallise if you wish.

Has anyone attempted this before? Please let me know if there are any potential problems with this method?
 
Yeah I was talking about this the other day on the chat, someone asked if it was possible to extract in a way very similar to what you described. I also wonder if it would work!

Two changes I would do would be to first of all thoroughly filter the acetone pulls before doing FASA. Also the freebasing step I would not do as you described but rather as it is described in BLAB, the slow water crystallization using sodium carb.
 
endlessness said:
Also the freebasing step I would not do as you described but rather as it is described in BLAB, the slow water crystallization using sodium carb.
Click to expand...

Thanks I was just thinking of how to do it off the top of my head, Im sure there are some more efficient methods of freebasing the fumarate salt such as the one you just mentioned. Thanks I will go check that out now!

Also would there be a way to regenerate the FASA back into reusable acetone, add sodium carbonate maybe? This would produce sodium fumarate which hopefully would precipitate out of the solution. But then again water would be produced as a product. Maybe the acetone would simple have to be thrown away, or could it be used for further pulls?

Thanks
 
hmmm thats an interesting question.. Indeed it would use up a lot of acetone.. Would be interesting to test your idea of sodium carb... The other option would be distilling, though its not for everybody. But considering acetone's really low bp, maybe a simple distilling scheme can be made, like a pot with a glass-only top upside down (so that the condensing acetone drops to the middle), and a little glass in the middle to collected distilled acetone.. This can simply be put in the sun (maybe I can find a scheme to help explaining). I would like to try that sometime see how well it works. Some water could also come over but then acetone could be further dried with magnesium sulfate or something similar, at least to an acceptable degree.

What do you think?
 
EDIT: sorry didnt read you post properly you already suggested a drying agent, we must think alike :)

Just had another idea, you could dry the acetone with anhydrous Calcium chloride (or a similar drying agent) then filter the mixture to remove the hydrated CaCl2 and the Sodium Fumarate. In theory what you would get is just acetone. If you used an excess of sodium carbonate that would ensure that the pH of the acetone remained above 7, so the solvent would be suitable to re-extract more freebase.

The extra work of regenerating the acetone would mean that probably no more that 2 pulls would be done with one batch of acetone. Although, acetone is so cheap compared to other np solvents like d-limo that it wouldn't matter that much if you threw it away after the second pull.

You could follow these (theoretical) steps

Pull 1 with fresh acetone 100ml ---> Salting ----> wait for precipitate

Pull 2 with fresh acetone 100ml ---> Salting ----> wait for precipitate

Pull 3 with fresh acetone 100ml ---> Salting ----> wait for precipitate

(all these pulls could happen pretty much simultaneously) Numbers are abitary i only chose 100ml because it is an easy number to work with


Collect all the DMT fumarate and freebase it using desired method

Treat the ~250-300ml FASA (some will have naturally evaped) with sodium carbonate, dry and filter to get acetone

Pull 4 *final pull* use the regenerated acetone to do a final pull, there will be less DMT available anyway now. ---> Salt ---> freebase

or if you are feeling lazy, do not salt, Evap for crude freebase product (wash with cold water to remove sodium and fumarate ions), which you could either use to make enhanced leaf or you could recrystalise with naptha for a cleaner product.

The acetone would probably have some Na ion and fumarate ions in it, but it shouldnt make too much of a difference.

This needs to be tried out.
 
Would like to say thank you endlessness for your contributions so far. It would be much appreciated if you could post up those plans for a basic still. Also I have been noticed that this theoretical tek is quite similar to the BLAB, except instead of d-limonene using only acetone. My only concern though is that DMT fumarate may be a little bit soluble in acetone because acetone is a little bit polar, certainly more polar than d-limo or xylene.

Do you have experience with using acetone? Ive read on the nexus wiki that it DMT is 'very soluble' in acetone, but does it pull full spectrum or just the n,n-dmt? SWIM prefers the n,n rather than jungle alkaloids.

Ive come across some inexpensive d-limo, so I might give the BLAB a go, and abandon this acetone idea. However, still I am curious to see how well it would work. Any thoughts or comments would be helpful

Thanks
 
Carrierwave said:
You will likely regret using Calcium Hydroxide. Stick with Sodium Hydroxide.
Click to expand...

Thanks carrierwave, I have used calcium hydroxide in the past in a standard acid/base freeze precipitation technique with naptha and it worked perfectly. But I understand that people have different reasons for using different bases. Is there any particular disadvantage of using Ca(OH)2 when working with acetone?

Thanks
 
Hey!

So I was thinking something using this principle:

Except not having a plastic top with coins to drop condensation, but rather some glass in a concave shape on top of a stainless steel pot (and doing with acetone not water, obviously). What do you think?
 
Thanks for posting that up, its a really nice and simple idea. Like you said, there would have to be no plastic in the design because the acetone would eat it up all too readily. My only concern about leaving a sealed container of acetone out in the sun for a long period of time is its low flash point, is there a potential for explosion?
 
Hi delta-9

the potential for an explosion is relatively low, because the temperature which is needed for selfignition is at 535°C. But who knows if UV light from the sun might interfere here?:shock:

I´m quite experienced with solvent redistillation (ethanol, naphta, petroleum ether boiling point 30-60°C and aceton) and I doubt that your/endlessness idea about using the sun as energy source would work properly.:cry:
The reason is that your temperature difference between the vessel and the lid is too little. The sunlight has to pass your glass lid and is heating it up too, so your condensation will take ages or at least one or two days. Evaporating during the day, condensing at night.
I use a waterbath on an electrical heatplate and icecubes in the lid (ss bowl). This way I need about 1 kg ice (perhaps a bit less) for 1 litre of aceton. The whole procedure takes less than an hour. And of course I´m doing this in a very good ventilated room, but when you have adjusted your heatplate properly you´ll have nearly no fumes in the air even in an open system.

In Lak´ech

Garfield

*edit*:
I reread your (delta-9) last post and figured that you want to use a sealed container.
Bad idea!!!
The selfignition temperature drops significantly when your aceton is under pressure. At 6.8 bar it is only 265°C.
On the other hand the fumes can only explode between 2.2 and 14.3 Vol.%.
But the risk of an explosion would be too high in my opinion.
 
Hmmmm interesting, thanks for thinking with us :) I indeed dont know if it would work in practice, im just thinking out loud here, would be cool to find something easily doable for basically anybody... Garfield, you say the difference in temperature wouldnt be so big, but what if you paint the outside of the pot black or you have some black material around to absorb heat on the sides, and on top you put ice? And/or what if you have it on top of a glass table (or improvised one) with a mirror below to reflect more heat to the bottom of it too?

Yeah a safe hotplate in a well ventilated area and all precautions sounds great, Im just wondering if one could do it with kitchen/home materials (or cheap/easy enough to find) instead, but maybe not possible.. What do you think?
 
endlessness said:
Hmmmm interesting, thanks for thinking with us :) I indeed dont know if it would work in practice, im just thinking out loud here, would be cool to find something easily doable for basically anybody... Garfield, you say the difference in temperature wouldnt be so big, but what if you paint the outside of the pot black or you have some black material around to absorb heat on the sides, and on top you put ice? And/or what if you have it on top of a glass table (or improvised one) with a mirror below to reflect more heat to the bottom of it too?

Yeah a safe hotplate in a well ventilated area and all precautions sounds great, Im just wondering if one could do it with kitchen/home materials (or cheap/easy enough to find) instead, but maybe not possible.. What do you think?
Click to expand...

The way with a black pot and ice on top should work, also your idea with a mirror, but you´ll need a lot of ice, because the sun will melt away a good portion of it. :cry:

I´ll start a new post about solvent re-distilling with some pictures of my "aparatus" during the next days. Btw it can also be used as a soxhlet.:d
 
Hi garfield, thanks for your contributions.

Garfield said:
I reread your (delta-9) last post and figured that you want to use a sealed container.
Bad idea!!!
The selfignition temperature drops significantly when your aceton is under pressure.
Click to expand...

This was my concern, hence why I was doubtful of the safety/effectiveness of the proposed technique.

If the container was sealed there is risk of explosion or auto ignition. However if the container was unsealed, the acetone would rapidly evap on a sunny day, making the whole exercise pointless. Ideally a distillation column would have to have something cooling it, ice is a good idea but it would melt quickly. Leaving it out in the sun seems a bit of a crude method because there is no real ability for temperature control.

Thanks
 
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