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Old 01-07-07, 22:24   #1 (permalink)
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DMT recrystallization TEK

I have had some trouble finding a comprehensive recrystallization TEK, so I have put one together based on my experiences in recrystallization. I used some tips from marsofold and vovin and added my own techniques.

I am only a second-year biochem student, so I have a few questions for you real chemists, and they will follow the TEK in this post. I would also like to know what my fellow DMT extractors think of my TEK. So, here it is:

The Entheogenist's DMT recrystallization TEK

What you need:

-- 3 one-pint mason jars

-- Naphtha (Ace brand VM&P Naphtha)

-- a small (1mL) buret to separate the layers if a sep funnel unavailable. (a turkey baster is too big, and is not effective for separating layers.)

-- large glass evaporating dish

-- Crock pot

-- Filter papers and a funnel (a vacuum filtration system is preferred and will improve your yield, but if you don't have the 50 bucks to drop, the cofee filter and funnel are fine.)


First, weigh your DMT on a digital scale accurate to at least .01 grams. You need 70mL naphtha per gram of DMT, so multiply the figure from the scale by 70, and that is how many mL of naphtha to use. Measure out the naphtha and place it in a mason jar.

The naphtha needs to be hot in order to dissolve the DMT, so we have to use a water bath, since naphtha is VERY flammable.
Fill your crockpot with enough water so that when you place the sealed mason jar in the water, the level of the water is half an inch or so above the level of naphtha. If the jar floats in the water, it's okay.

Remove the jar from the water while heating. No need to heat the water to boiling, just piping hot. We don't want to get it too, hot, since the naphtha is in a sealed container. When the water is hot, place the naphtha jar in the water for 15 minutes.

While the naphtha is heating, sprinkle the DMT powder on the bottom of the second mason jar. After the naphtha is heated, pour it into the jar with the DMT and seal the jar. Swirl the liquid around until all the DMT is dissolved.

While it is cooling, tilt the mason jar to the side. You will notice a small layer (more like a puddle) of impurities collecting in the corner of the jar. (These are probably tannins or oils from the root bark, along with dust from the air, and possibly some of the basified material from the extraction that made it into the final product due to the slightly sloppy lab technique displayed by some of us kitchen chemists.) Use your buret to reach down to the bottom of the jar and suck that oily layer out of your solution, and place it in the other mason jar.
If no bottom layer forms at all, that's fine. It just
means you did a great job on the initial extraction.
Note: If a buret is not available, you can pour the solution into a ziplock bag, pin the top corner to the wal, and let the oily layer collect in the corner of the bag. Make a pinhole in the corner to let the nasty layer drain out.

Let the solution cool to room temperature.

Place the solution in the refrigerator for 24 hours, then place it in the freezer for 4 hours, and then in the fridge again for 4 hours. Each time you alternate, swirl the solution around in the jar quite a bit, but don't shake it and don't let it get too warm. Alternate between fridge and freezer every 4 hours during the day, and leave it in the freezer for the night. Do this for at least 2 days. . The longer you carry on this process, the bigger the crystals will grow. Alternating between cold and cool allows the crystals to grow bigger and purer by partially dissolving the crystals then reforming them each time you switch from fridge to freezer. When you are finished, let the solution sit in the freezer for 6 hours.

Prepare your filtration system before removing the jar from the freezer. Fold the filter paper into a cone shape that fits in the funnel. Place the funnel in the third mason jar so it stands up. Have a couple premade filter cones ready in case the first one gets clogged.

Remove the mason jar from the freezer, shake it up really good, and if there are crystals stuck to the bottom, use a piece of wire to quickly scrape them off a bit. Before the solution warms at all, pour it through the filter SLOWLY. If it clogs, remove the filter and use a back up cone. When it's all filtered, spread out the filter paper and let the crystals dry. This product is finished and ready for smoking.

If there are crystals stuck to the sides and bottom of the mason jar, pour the filtered naphtha into that jar and swirl it until it is all dissolved. You may need heat it again in the water bath. When it is all dissolved, pour the solution out on the evaporating dish, and let it evaporate in a well ventilated area, with no open flame.
When it is dry, scrape the crystals up and let them sit out for awhile to ensure they are completely dry, then you can mix them in with the rest of your crystals. This step ensures that you get every last bit of happiness out of the naphtha solution. You could evap the original solution without doing any freeze precipitation, but I prefer the freeze precip for the majority of the product. I just use the slow evap to wring out the last bit of DMT that didn't fall out in the freezer, and to get those annoying bits that stick to the jar after freeze precip.

Well, thats my completed recrystallization TEK. ENJOY!


OK, here are my questions:

If you are planning to recrystallize, is it necessary to do the ammonium hydroxide wash beforehand?

and,

Can anyone provide a definite TEK on extracting the "red jungle DMT" from mimosa? I am fascinated by this mystery compound, and would like to explore it. Does anyone know if the compound has been identified or if it is orally active?

Well, much love to the mycotopia community and a big thanks to marsofold and vovin for enhancing my life with their easy to understand TEKs.

PEACE!
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Old 01-07-07, 22:48   #2 (permalink)
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Old 01-07-07, 23:24   #3 (permalink)
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'Red jungle DMT', as it has been called can be extracted using Xylene as a nonpolar solvent. The final extract could be washed with naptha (which would be evapped to give dmt) to yield 'clean' 'jungle dmt'


also, heptane/bestine or any number of other solvents are better than naptha for recrys..but this is a pretty good tek.
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Old 01-08-07, 22:52   #4 (permalink)
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Thanks for the input.

So, does anyone know if it is necessary to do the ammonia wash to clean the DMT before recrystallization? Would the recrystallization process serve the same purpose?
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Old 01-09-07, 16:57   #5 (permalink)
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Recrystallization makes the ammonia wash unnecessary.
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Old 01-09-07, 19:30   #6 (permalink)
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Sweet. Thanks so much for sharing the knowledge.... this clears things up a lot for me.
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Old 01-10-07, 16:41   #7 (permalink)
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One more question:

Will freeze precipitation work with the xylene? Or do I have to evaporate it? If freeze precip works, will the jungle dmt and regular dmt both fall out?
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Old 04-20-07, 23:29   #8 (permalink)
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I cannot believe people are still using my old tek. God this is a bast from the past.
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Old 04-21-07, 07:10   #9 (permalink)
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Right on Vovin !! your web site was great too !!

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Old 04-22-07, 15:17   #10 (permalink)
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Quote:
Originally Posted by vovin View Post
I cannot believe people are still using my old tek. God this is a bast from the past.

what is your most current tek? can you post it here?
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