Advice for converting Fumarates to Freebase

[brand_new_bein]

I have some questions about the best way for converting DMT-Fumarates to Freebase given my situation.

I did an STB tek on 100mg MHRB and yielded about 1.3g and change after 5 pulls from naphtha. I lost some of the yield due to some mistakes in doing a wash and some while evaporating, so I thought to do a 6th pull of Xylene to get some more spice from my Lye juice to recoop my losses. I also wanted to learn more about the FASA method and converting Fumrates to freebase which I am planning on doing now.

Doing FASI on about 80 mL of Xylene pulled from the Lye MHRB Soup precipitated some creamy crystals and some orange goo on the sides and bottom of the beaker. I let the solution precipitate for over 24 hours and after not getting any clouding upon adding more FASI I decanted through a filter and put the beaker upside down on an evap dish to dry.

A while later I noticed that the orange goo had dripped into the evap dish while the crystals remaind stuck to the beaker. So now I have what I am assuming to be DMT-Fumarates in two different places making it hard for me to weigh or store in the form they are in. At this stage I would like to convert all of this to freebase to be able to measure what I yielded from the last pull and possibly smoke the product which as I understand might contain trace alkaloids pertaining to the infamous 'jungle spice'.

So I'd like to know from those more experienced with goo fumarates and precipitation what is the best way forward. I am assuming there is 0.4-0.5g of Fumarates there but I have no way of knowing because can't get the goo on the weigh scale.

If I disolve all of this in warm water to get it back in one container, how much watter should I use?

Then once I have all the fumarates disolved in water, what is the best way to get freebase? Is it to evap the water get the dried frumarates and do a paste n' pull technique with 1:1 sodium carbonate and minimal water then pull with acetone three times and evap the acetone. One problem with this is that I might get a goo again upon evaporating and then how to go about making a 1:1 paste?

Or should I use the DMT-Fumarate water as is and add saturated sodium carbonate water solution drop by drop to get cloudy precipitation going and then refrigirate it and decant the liquid after a few days and hopefully retrieve the cryztals from the bottom of the jar. A problem here is the solution might not precipitate fully, or I might end up with some indecipherable sludge or goo and some of the freebase might be in the liquid still.

Anyway I would like to do this in the simplest way possible avoiding any mess ups, so any adivice anyone can give looking at the attached picture of the fumarates I have on hand, please suggest what is the way to go so I can begin the next step of the process. Thanks for all your help on this front. Cheers!

 

[Ruffles]

There are conversion teks in the wiki, you should read them all and make sure you understand the principles. Be prepared to lose some weight due to less fumarate and due to the process itself, but its worth it.

To answer some of your questions: If you have dry fumarate, keep it as such until you are going for freebase conversion, that`s the most stable form of DMT. Acetone is not a good choice to manipulate-wash freebase in my opinion. If you already dissolved fumarates in H2O, you might add carbonate (at least equal weight to fumarates) and then follow up with a two-phase liquid separation (just read below), but I believe that paste-n-pull is probably easier to manipulate because of the smaller volumes overall. Jungle spice (yellow or red stuff) is not really a problem for DMT consumption and effects. Xylene grabs yellow and red stuff which you won`t really be able to separate without recrystallization in a different solvent like hexane, you are going to lose white stuff while trying to lose the yellow red. Your fumarate crystals and yellow water looks fine and clean enough, don`t expect the white perfection without more steps that costs yield.

This is how we do it: Add 1:1 weight (that`s 1 g NaHCO for each 1 g Ds, you can safely add a bit more carbonate, like 1.3 g for 1 g) of sodium carbonate powder on top of your dried fumarate, mix well. Put it in a flat glass container that you can fit your hand on to easily handle the mix, like a glass petri dish. Add water bit by bit, add some, mix, add more, mix... do that until it turns into a paste. Wait 10 min or so for the high pH to convert fumarate to freebase. At this point you might see a brownish residue either stick to the glass or rise up, that`s most of your freebase. Then comes the tricky part, which is separating the freebase from water and sodium and fumarate (the components of the mix). If your freebase brown gunk coagulated enough and is stuck in the glass you can just add cold water drop wise and tip the glass plate, collect the water that comes down until you see that whiter stuff not near your gunk, that would be washing.

However, and here is my advice: in our experience freebase doesn`t coagulate or stick to the glass well. The way we do it at this point feels easier, which is basically a two phase NPS-water separation: just grab all the water and white and gunk and put it into a tall skinny glass, then you add a small amount of your low evap temp NPS (hexane, dcm, xylene, check DMT freebase solubility to know exactly how much NPS to add) and add to water-gunk-fumarate-carbonate water, do a shake and decant off the polar-water unwanted stuff, freebase goes into NPS (you may do 2 pulls to make sure to grab all). We do a second wash on the NPS, by adding clean water that has a pH of at least 9 or higher and doing a shake. Then we grab the NPS and put it on the evaporation dish (glass petri dish or similar) and after NPS is gone you can cut it with a razor blade. It comes out fumarate and sodium and carbonate free. Should look transparent after dried and then white to yellow after you cut it.

 

[Dirty T]

I've never had any luck using sodium carbonate to convert a backsalt before, the PH is too low. Ive always just based with Sodium Hydroxide. I tried soda ash before but like I said, it didn't work very well. You may try using larger volumes to minimize loss, I know that sounds backward but there is a sweet spot between not enough and too much volume for a given amount. It is a lot easier for me to pull a gram of DMT from a liter of liquid using 100ml solvent than it is trying to pull 1g DMT from 2ml liquid with 5ml solvent as an example.

Quick story. I had some Xylene I was evaporating covered with a paper towel over the weekend. On Sunday I found the paper towel in the dish and crusted over hard with DMT. I simply took the towel, washed it in clean Naphtha, threw the Naptha in 300ml Acetic acid, shook and applied heat for 10 minutes, based it and collected 2.5g DMT in less than an hour. I could have skipped the first step and threw the whole paper towel in my Pyur bottle but I don't want to dig little bits and pieces out later.

** Edit - SODA ASH SHOULD WORK FINE FOR THESE PURPOSES. IT HAS A PH OF 11.4 AND ALL DMT IS CONVERTED TO FREEBASE AT 10.68. WHATEVER THE REASONS FOR MY FAILURES IN USING IT MUST BE MY OWN FAILURES. UNLESS SOMEONE CAN CORRECT ME MY ORIGINAL STATEMENT IS INCORRECT AND SODA ASH IS A VIABLE BASE FOR CONVERTING NNDMT ACETATE TO FREEBASE.

 

[brand_new_bein]

There are conversion teks in the wiki, you should read them all and make sure you understand the principles. Be prepared to lose some weight due to less fumarate and due to the process itself, but its worth it.

To answer some of your questions: If you have dry fumarate, keep it as such until you are going for freebase conversion, that`s the most stable form of DMT. Acetone is not a good choice to manipulate-wash freebase in my opinion. If you already dissolved fumarates in H2O, you might add carbonate (at least equal weight to fumarates) and then follow up with a two-phase liquid separation (just read below), but I believe that paste-n-pull is probably easier to manipulate because of the smaller volumes overall. Jungle spice (yellow or red stuff) is not really a problem for DMT consumption and effects. Xylene grabs yellow and red stuff which you won`t really be able to separate without recrystallization in a different solvent like hexane, you are going to lose white stuff while trying to lose the yellow red. Your fumarate crystals and yellow water looks fine and clean enough, don`t expect the white perfection without more steps that costs yield.

This is how we do it: Add 1:1 weight (that`s 1 g NaHCO for each 1 g Ds, you can safely add a bit more carbonate, like 1.3 g for 1 g) of sodium carbonate powder on top of your dried fumarate, mix well. Put it in a flat glass container that you can fit your hand on to easily handle the mix, like a glass petri dish. Add water bit by bit, add some, mix, add more, mix... do that until it turns into a paste. Wait 10 min or so for the high pH to convert fumarate to freebase. At this point you might see a brownish residue either stick to the glass or rise up, that`s most of your freebase. Then comes the tricky part, which is separating the freebase from water and sodium and fumarate (the components of the mix). If your freebase brown gunk coagulated enough and is stuck in the glass you can just add cold water drop wise and tip the glass plate, collect the water that comes down until you see that whiter stuff not near your gunk, that would be washing.

However, and here is my advice: in our experience freebase doesn`t coagulate or stick to the glass well. The way we do it at this point feels easier, which is basically a two phase NPS-water separation: just grab all the water and white and gunk and put it into a tall skinny glass, then you add a small amount of your low evap temp NPS (hexane, dcm, xylene, check DMT freebase solubility to know exactly how much NPS to add) and add to water-gunk-fumarate-carbonate water, do a shake and decant off the polar-water unwanted stuff, freebase goes into NPS (you may do 2 pulls to make sure to grab all). We do a second wash on the NPS, by adding clean water that has a pH of at least 9 or higher and doing a shake. Then we grab the NPS and put it on the evaporation dish (glass petri dish or similar) and after NPS is gone you can cut it with a razor blade. It comes out fumarate and sodium and carbonate free. Should look transparent after dried and then white to yellow after you cut it.

Thanks for all the useful advice. I have read many of the teks and somewhat understand the principles behind backsalting and freebasing.

1: I don't mind the yellow, red or brown stuff. I know it comes from the plant fats and other ingredients. As long as its safe to smoke its fine by me, I am not a crystal purist or looking for the whitest stuff possible. Have had some powerful experiences from brown goo so that's fine as well. Just looking to keep most of the yield in tact, so trying to go with the least messy way.

2: Because some of it is goo and some of it is crystal, I cannot weigh it to be sure what the exact quantity of sodiumcarb to add to base it via paste n pull technique. So I am considering maybe disolving it all in water and then drying it on a petri-dish and then evaporating to see what I end up with.

3: As you said, fumarates are more stable than freebase so may make sense to store them as such. I could combine these with other fumarates I may get from future extractions and then freebase when I need, as I have plenty of freebase from the earlier part of the extraction to go by for a while. But to store these I would like them to be more powdery and less gooey, is there a way to evap them in such a way as to make sure i get less goo in the end?

4: At some point I would like to try pharma, combined with harmala extracts. So I am wondering if the fumarates I have are food-safe, given they have been extracted with Xylene (which is known to be toxic). I have been drying them for a couple of weeks so not sure if traces of xylene are still in the goo. If these are not orally administrable than I'd be more inclined to freebase them.

5: If I follow your advice, which seems sensible and reasonable, then I have a couple of other questions in what you stated. What NPS can I use for the 2-step process, I am afraid if I use the Xylene again I would have just gone round in a circle and have to evap this disgusting liquid down with a chance of making a mess. If I use Naphtha, I might be loosing some of the more 'jungle' bits of the spice? - this is fine too though. I am not sure if i can find heptane or hexane at this point. I have Naphtha, 99% IPA (which i know disolves in water so not good for sep), and 99% Acetone (which the paste and pull tek advises to use but you advise against.

6: Correct me if I am wrong, you suggest add clean water with pH of 9 or higher, that would make it basic water so how can it be clean and basic for this step to work?

7: Re: DirtyT's point about soda ash not being a good base. I have Sodium Hydroxide as well, would that work as well for the basing step or does it have its disadvantages?

Thanks for all your help! I know a lot of this info is out there already but piecing together all the info with all the contradictory bits can be confusing as hell to a non-chem noob. So appreciate the advice very much

I'll try to get some petri dishes in the mean time

 

[Ruffles]

Hey, we had the same problem during reading of the conversion teks, totally understand the derived confusion.

1 - in our experience, when you grab fumarate DMT and convert to freebase like described it comes out very much ok to smoke. Just make sure you dry as much as possible of the NPS, oven dry, then cut, oven dry a bit again. You can tiny taste it to feel the difference between partial and fully dried freebase.

2 - you can just guess how much there is in that small amount of liquid and go for double the amount to be sure you convert most (guessing 100 mg is in there, put 200 mg sodium carb), the excess sodium will mostly stay in the polar phase, not the NPS.

3 - for the fumarates, we decant off the NPS then put the glass and crystals stuck in its surface into an mildly warm oven (50 celsius or even more), it certainly evaps 99% out of xylene in an hour or two, and the fumarates can take it (would go for 50 celsius tops to dry the freebase). Don`t leave it lying around for a week or so in contact with air and room temperature (maybe that`s what made it more gooey), you should dry and cut as fast as possible. A second option for getting the goo out would be boiling IPA dissolving and then cold recrystallization of your dry fumarates, its wonderful and easy to clean up fumarate DMT, it could separate somewhat the goo from the yellow or white DMT. Has to be 99%-100% IPA though.

4 - see answer 3. Word of advice: crystals will retain some NPS solvent into it regardless, but its a tiny amount that can`t really intoxicate your GI tract all that much. It won`t ever be approved by the FDA to be `food safe`. Fumarate DMT from xylene tastes like xylene, from hexane tastes like hexane, and so on... that`s inevitable. Boiling IPA recrystallization improves immensely the taste of fumarates. Smoking is another matter.

5 - you can do hexane or naphta to grab the converted to freebase DMT from your polar phase, it should evap better than xylene as it takes less heat to evap. Naphta and hexane though, I believe its required to be warm to grab freebase DMT. Xylene doesn`t. Either way, you should evap better with heat (40-50 celsius). Since you are smoking it which is more sensitive to fuck ups, well you won`t be able to avoid it but xylene and hexane like I said before will be in the crystals in a tiny amount. IPA and acetone won`t phase separate, can`t be used, has to be non-polar.

6 - Clean water pH 9 for the washing of the NPS with your converted freebase, that is, decant off the water with carbonate and sodium, add more pH 9 water, another shake and decant that off too. That grabs most of the sodium that would be left in the NPS out of it. pH 9 water is clean in the sense that it has much less sodium compared to the previous water, loaded with NaOH or sodium carb from your conversion. It doesn`t take much NaOH to get water to pH 9.

7 - I think NaOH can be used, but its a stronger base, and if I understand it, sodium carbonate is a weaker base and `food-safe`. Don`t know how much to add of NaOH though (1 g to 1 g estimated DMT?). Couldn`t be that much of a problem.

Petri dishes or flat pyrex dishes, whatever, needs to be flat and fit a hand with a flat blade to cut the thing.

 

[Ruffles]

From a different post, downwardsfromzero gave a great idea as a cleanup of freebase to remove residual NPS, which is to dissolve the freebase into ethanol and evaporate it (which for me means to heat dry-cut-reheatdry).

 

[Dirty T]

I am sorry about my previous post. NnDMT has a PKA of 8.68 and sodium carbonate has a PH of 11.4, at 10.68 all DMT-acetate is converted to freebase so it can definitely be achieved through Soda Ash. I personally wouldn't worry about food safety, NaoH is also used to make pretzels among other food products. If everything is performed correctly there shouldn't be any residual NaoH. Ethanol or IPA are also good easy effective ways to clean up. For your question about NPS I always use Naphtha to pull after backsalting Xylene (after I evaporate any residual Xylene BEFORE basing because getting Xylene in the mix prevents freeze precipation in my experience) with minimal to no loss.

I apologize for the earlier interruption of your thread and the misinformation I posted. Whatever caused me to fail when I tried using soda ash for conversion must have been my own fault. Soda Ash should be a viable method to convert nnDMT acetate to freebase NnDMT.

 

[downwardsfromzero]

Whatever caused me to fail when I tried using soda ash for conversion must have been my own fault. Soda Ash should be a viable method to convert nnDMT acetate to freebase NnDMT.

Soda ash will slowly absorb carbon dioxide from moist air to form sodium bicarbonate. Maybe your soda ash was a bit old, and had been stored in a less-than airtight container? It may be prudent to toast one's soda ash in a stainless steel pan or blast it in the microwave a bit before each use. This should help it maintain its basic potency by decomposing any bicarb which may have formed during storage.

 

[brand_new_bein]

I disolved all of this goo and crystals lining the beaker in hot water and re-evapped on some petridishes to get some scrapable product. problem is much of the goo is still quite gooey even afer heat evaporation. ive measured the entire fumarates extracted from xylene to be about 0.5 grams. I am wondering if it would be safe to eat some of these fumarates as a dose of pharma with some harmalas. Or should i try to clean them up further before consuming. What would a good and safe amount be to take in order to test if its active as DMT?

Or should I try converting all of this product to freebase and see what I end up with?