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chemist1243
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[*] posted on 5-9-2019 at 06:37
DMT extraction.


Okay, so I wrote this extraction up just to exercise my current knowledge
Of acid-base extractions. I first learned about how to isolate alkaloid from impure products somewhere around may of 2019. Acid base extractions are extractions that use the alkalinity, acidity, and polarity of a desired compound to isolate it from impure sources such as plant matter.

This is extremely useful for chemists like me, whom are interested in getting raw material from nature and it counterparts.
Now of course, there are plenty of other people who have formulated methods to get DMT. this is just my personal method that I created based on my current knowledge of chemistry. I'm sure there are many others just like mine, so I made sure to not research them so that I can challenge myself to figure it out completely on my own.

Also, i was board, so ya know, i thought making this would be fun.

So without further explanation, I present, the extraction of
N,N-Di-methyl-Tryptamine from mimosa hostilis root bark:








































This is a theoretical extraction. Recreation of any actions described below can result in legal trouble and/or chemical burns. Do not attempt to create DMT or its analogs. DMT is a schedule 1 controlled substance, making its manufacture and possession illegal and punishable by law. This is for demonstrative purposes only.

Chemicals needed:

50g mimosa hostilis root bark

200g sodium hydroxide(lye, caustic soda)

800ml distilled water

10ml 31.45% hydrochloric acid

550ml of naphtha









Equipment needed:

250ml separatory funnel

Hotplate

2 250ml beakers

Rubber band

Plastic bag

1000ml RB flask

Reflux condenser

250ml flask









Safety concerns:
Naphtha is flammable, so keep away from flame. Hydrochloric acid and sodium hydroxide are both extremely corrosive, so wear gloves, long pants and sleeves, and definitely wear safety goggles. . Always follow proper lab procedures regardless of what you are doing.

PROCEDURE:

100g of sodium hydroxide is dissolved in 500ml of water. This is added to a 1 liter RB flask along with 50g of finely shredded or ground mimosa hostilis root bark. Thoroughly mix the root bark in. reflux this at around 50 degrees celsius for 12 hours.

After two hours of reflux under extremely basic conditions, you can kill the heat and allow the solution to cool.

Listen carefully to this step. Once the solution has cooled, add 200ml of naptha. Shake the solution so that the naphtha layer gets evenly distributed throughout the mixture. Now set it up to reflux just barely above room temperature, around 29-36 degrees celsius. Reflux the mixture until the naphtha floats back to the surface of the liquid to form a separate layer. After the naphtha has separated, shake the flask again to redistribute the naphtha through the solution. Set this to reflux at a warm, NOT HOT, temperature until the naphtha forms a separate layer. Repeat for 24 hours.

After 24 hours, add the entire solution to a separatory funnel. Try not to get any plant matter into the funnel, because it will clog it up. If you are using a 250ml funnel, you will have to do two runs. Okay so after it has been transferred to a funnel, allow the naphtha layer to completely separate from the aqueous layer. Discard the sodium hydroxide layer. Optionally, you can dry the naphtha with saltwater solution.

Anyways, now you need to let the naphtha layer evaporate.
Put it in a bowl or dish and allow the naptha to evaporate until you are left with dry, solid crystalline material.

Crush up the crystalline material and add it to 200ml of water in a 250ml erlenmeyer flask. Acidify the water with hydrochloric acid while swirling. Add acid until the solution turns blue litmus paper dark red, indicating it is highly acidic.




Swirl the flask until either all or a majority of the DMT dissolves. What were trying to do is convert the DMT freebase into DMT Hydrochloride. This will cause it to become polar, allowing the DMT to only dissolve into polar solvents such a naphtha. The impurities, however, will only be soluble in non polar solvents.

Now we extract any residual fats, oils, and impurities. This is done by adding the acidified DMT water to separatory funnel along with 100ml of naphtha. Shake gently for 5 mins and discard the naphtha layer. Repeat once more with 50ml of naphtha.

If you have done everything correctly, you will now be left with about .5 grams of pure DMT hydrochloride dissolved in water. Dissolve 100 grams of sodium hydroxide in 200ml water.
Add this to the DMT hydrochloride solution until a PH of 10-14 is achieved. Once it has been basified as necessary, swirl in an erlenmeyer flask for 5-10 mins.

Reflux with 200ml naphtha at warm temperatures for 24 hours. Collect the naphtha using a separatory funnel. Evaporate the naphtha to yield 100% DMT freebase.


Here's what's happening. The naphtha is nonpolar, therefore it cannot dissolve in the sodium
hydroxide solution. The freebase DMT, however, is nonpolar, so it dissolves in the naphtha. For the DMT to actually dissolve, it needs to interact with mimosa hostilis root bark. when shaken, the naphtha is getting trapped below the mimosa hostilis root bark, and therefore it is forced to interact with it, thus dissolving DMT into the naphtha in the process.



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TheMrbunGee
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[*] posted on 5-9-2019 at 08:19


"Reflux" times are overkill, NaOH amount is overkill (actually amounts all seem quite high). You have written a very nice procedure, but it screams that you need more practice with simpler/cheaper extractions. You should do a few, and see what happens if you change things.

I think if you would have done this exact procedure, after all you could see how you could have used less solvent or less base (in this case it could actually decrease purity or even ruin the extraction). And do less "reflux".

But I might be wrong.




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Boffis
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[*] posted on 5-9-2019 at 10:56


Have you tried this and final what yield did you get? What sort of naphtha are you using, petroleum ether B. R. 30-60 C?

Why do you need so much sodium hydroxide for such a small amount of bark? And again when you free base the hydrochloride do you need 100g of sodium hydroxide? This is about 1000x the amount required!!! Using large excesses of reagents is like to reduce yield.

I suggest you use a lot less NaOH in the first plase, add the naphtha and proceed as you describe but then filter the whole lot, wash the cake with naphtha and then allow the filterate to separate; much clearer separation once you get rid of all the floaters and veggie crap. Remove the naphtha phase and concentrate somewhat then extract with a small valume of dilute HCl.
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draculic acid69
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[*] posted on 9-9-2019 at 18:31


I think if you change 200g NaOH to 20g it might be better.your using 4x the amount of your starting material which has only like 1% of the compound you have to p.h.
Definitely overkill on the amount
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[*] posted on 10-9-2019 at 00:36


too much sodium hydroxide, way way too much.
plus it is alaays better to do more extractions with less solvent than 1 extraction with half a liter of solvent, basic knowledge on phase repartition. reflux times also too long, by doing more extractions with less solvent the process is faster, higher yielding and at the end you have less waste.
your 100% yield is very optimistic hahahaha





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DrIronic101
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[*] posted on 16-9-2019 at 20:14


So what you're doing is the universal straight-to-base extraction, with a re-extraction at the end, sounds like. A few points:

1. WAY too much NaOH. At most 50-75g is all you'll need for this.

2. Schultes gives the percentage of N,N-DMT in Mimosa hostilis root bark to be around 0.31% to 0.57%. This means that a 100% yield would be anywhere between 185mg and 285mg. Never expect a 100% yield, because you will be disappointed. Around 80% is a good target to shoot for. This would mean a yield of between 148mg and 228mg. The actual product will weigh slightly more but Mimosa hostilis extract is a wide variety of other compounds-- expect at MOST 500mg of product.

3. Reflux times are excessive. For the record, reflux is hardly necessary at all. You could just heat the solvent up to 50°C for a few hours and then let it chill out and do its own thing for 24 hours. That would be far more reasonable.

That's what I have to say.

~Ironic
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Sathariel
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[*] posted on 20-10-2019 at 17:53


I hope this isn't considered necroing, being the thread is a month old

I admire your enthusiasm and the time and effort you put into writing this up.
At any rate, I have quite a bit of experience with this.

As has already been pointed out by other posters, way too much NaOH.
A general rule of thumb that is almost guaranteed to provide a good yield is 1:1 ratio of NaOH:MHRB. For every gram bark, one gram NaOH. Add in the water and the ratio would be 1:1:25(ml); 25ml per gram:gram.

I don't explain things well, I hope you understand what I mean.

Skip the refulx.
If you used powdered root bark, as would be purchased for dye making, skip the heating/boiling as well.

(as an aside If you have chunks or coarsely shredded bark, an acid/base extraction would provide better results with less initial contaminants before any purification steps. Less chemicals would be used as well. Instead of adding enough NaOH to destroy the plant material, you would only need to have enough to bring the ph up to a certain point.)

I have used several different methods and have found that STB is easier and the slightly higher yield afforded by an a/B isn't worth the extra steps.

I have also experimented with ratios and found that 1:1:25ml works well, you don't even need that much NaOH or even that much water either.
The very last extraction that I did, the results of which I was very proud, the ratio was 1:0.5:9ml

Doesn't sound like it would work does it? I had gradually reduced that amount of water used over several extractions because processing that amount of material became a big pain. A big, messy, clothes-dissolving pain.

For every gram of root bark (powdered) 0.5 grams NaOH and 9ml water.
No need to heat or refulx. Just let it sit overnight; about 6-8 hours. If you start in the morning, shake the container every hour or so.

3ml naphtha (or toluene, xylene, limonene) for every gram of root bark, split into 3 portions for 3 pulls.
Non polar solvent should be room temperature.

Filtering powdered bark sucks. You can if you like. I did in the beginning but realized that it doesn't matter.

1 pull, 2 pull, 3 pull, add them together in a sep funnel. (Make sure the stopcock is closed)

Now time to wash your solvent.
Add a pinch (like, a gram or less) of calcium carbonate to a half of a volume of water and add that to funnel. Twirl end over end (don't shake) and don't forget to vent!

Discard bottom layer, drain top layer into a flask.
Now time to dry the solvent.

Obtain some dehydrated MgSO4. Add that to the solvent and swirl around until it no longer clumps.

Filter the drying agent out and add solvent to something with a lid.
Put that bad boy in the freezer over night.
Filter out crystals.







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chemist1243
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[*] posted on 21-11-2019 at 11:30


Quote: Originally posted by draculic acid69  
I think if you change 200g NaOH to 20g it might be better.your using 4x the amount of your starting material which has only like 1% of the compound you have to p.h.
Definitely overkill on the amount


yeah, i guess i kinda went overkill on the NaOH. it would probably make my yeild really large, but very dilute.
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XeonTheMGPony
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[*] posted on 21-11-2019 at 16:05


Quote: Originally posted by chemist1243  
Quote: Originally posted by draculic acid69  
I think if you change 200g NaOH to 20g it might be better.your using 4x the amount of your starting material which has only like 1% of the compound you have to p.h.
Definitely overkill on the amount


yeah, i guess i kinda went overkill on the NaOH. it would probably make my yeild really large, but very dilute.


Not really, just wastes materials and makes down stream tasks more tedious
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[*] posted on 21-11-2019 at 23:43


Mechanical loses from high volumes of liquid would be the primary factor affecting yield I'd imagine.
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stoichiometric_steve
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[*] posted on 30-11-2019 at 04:43


Quote: Originally posted by Sathariel  

A general rule of thumb that is almost guaranteed to provide a good yield is 1:1 ratio of NaOH:MHRB. For every gram bark, one gram NaOH.


I'm a little rusty on my stoichiometry, but that is still overkill as fuck. One gram of NaOH has so many -OH's, even with a crazy amount of polyphenols or other acids in the plant material, you're highly unlikely to exhaust the -OH's. And of course it'll have to be neutralized at some point, at least before disposal.

I'll post a proper soxhlet & liquid-liquid extractor based writeup soon.
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