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Fumarate to Freebase Question

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Ethnochemist

Rising Star
So swim followed the basing technique in the pdf given here.

7) dissolve the alkaloid-fumarate salts in 5ml of tap water, then and then add saturated sodium carbonate to make the solution basic. The alkaloids will be freebased and the solution will become milky. In 3 days they will precipitate out forming nice needle-like crystal in the basic solution. At this stage, one can filter the solution (nasty procedure since the crystals tend to be sticky and waxy) and retrieve any left alkaloids by dissolving them in acetone.

SWIM's just curious. He mentioned this in another thread, but just wants to provide background for this one. He dissolved about 1 gram of fairly pure dmt-fumarate in approx. 25ml of warm tap water. He then mixed 2 grams of sodium carbonate into 15ml of tap water and added that to the fumarate solution.

NOTE: The dmt-fumarate still smelled mildly of xylene, so there are definitely traces of it in the solution (swim probably should have done more acetone washes).

The solution was at first, as expected, very milky. But after 1 day, the crystals don't look like something recognizable. On the bottom there are brown blobs that resemble caviar. The solution is a little bit clearer, these blobs are growing on the sides of the test tube and seem to just float in solution, swim's wondering if anymore will even settle. As a test, swim took a spatula and scraped some down the side of the tube, they didn't move very much. The spatula was taken out and had very sticky/slippery liquid on it, after about 10 min, it was much drier and there was a considerable amount of crystals on the spatula.

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He should probably be getting needle-like crystals at least somewhat forming in the solution, but all swim is getting is these blobs. SWIM wants to wait one more day to see if more crystals will form and settle, otherwise he's moving to plan B, which invokes some more questions.

He wants to then just use a non-polar solvent to get out all the freebase. He has naphtha and xylene available to him at the moment. He wants to use naphtha because it's easier to evaporate (he doesn't want to use a freezer btw); however, naphtha does not pick up all the other alkaloids like J. Spice and the Oxides. But if he has to, he might have to use Xylene, but xylene is very annoying to evaporate...even if it's only ~100ml.

Worst case scenario is that he has to evaporate the Xylene (water bath, fan and all), which swim can deal with, but would prefer to avoid in all circumstances.

SWIM had one more question though. SWIM has 8um filter paper. It's been sitting for a day, so some crystals have formed, and swim assumes that almost everything should be bigger than 8um. Could swim just filter it now? (or tomorrow, giving it 2 days to crystalize). Then put the filter paper in the oven at 120F until the water goes away....then just run acetone through the filter? Hopefully the Na2CO3 will stay on the filter paper (actually, swim doesn't think it would matter anyway, Na2CO3 won't evaporate when vaporizing), and the goods come out the other side. SWIM has no problem evaporating acetone. SWIM's a little worried about the actual filtering. He doesn't have a vacuum, and swim is worried that toward the end it will be a large gel collection that won't filter through, meaning more oven time.

Thanks for the help,
E.C.
 
OMG, this method is stupid, SWIM's FOAF was never intending for this route to be widely used!

What he recommends is the sodium carbonate (or calcium hydroxide) / fumarates paste, as described in the tek.

What SWIY can do is get everything out of test tube and let dry completely. Maybe add some more sodium carbonate. Let everything dry completely (may take a day or 2), then pull the freebases with acetone leaving the crap (sodium carbonate, sodium fumarate) behind. Then, evaporate acetone to get the smokeable freebases.
 
Thanks for the advice.

So swim just added more base (should be a little over 1N now), an interesting thing happened. After shaking it, it became all milky again, but all the nasty orange oils floated to the top (xylene's fault?) and this very very white clumpy stuff sank to the bottom like a brick (hopefully it isn't sodium carbonate....but it's not dissolving and sodium carbonate's solubility is insane). Wonder what it'll look like later tonight.

The thing is...swim is kind of on a time schedule. Is there any way swim can harvest all these crystals in one day? Water evaporating will be quite lengthy. So here are swim's three options.

1. Filter the mess, dry the filter paper, run acetone through it.
2. Extract with xylene, evaporate xylene.
3. Put the 40ml of base water on a very wide pyrex dish and dry in the oven at 120F (swim's guessing that this could take several hours, might be faster than xylene though).

Which does swiy think will be the best?

E.C.

EDIT: SWIM's starting to like the water in the oven idea. It's the only way to ensure that swim gets everything back. Plus, it's 40ml spread out over a 9"x13" baking dish. Might go pretty quickly. SWIM will then just scrape up the solids, place it back in the test tube, and extract with acetone.
EDIT2: SWIM forgot that he had magnesium sulfate lying around (baked in the oven from Epsom salts). Could swim add that? He'd have to add ridiculous amounts, like 80grams to a test tube lol...but maybe he can add a little, then add the whole mess to the oven to make things dry faster. Or is dealing with MgSO4 when extracting with acetone harder (as in, the particles don't settle as fast or something).
EDIT3: Or, he could hijack a certain aspect of 69Ron's tek.... He could transfer the 40ml into a 500ml jar he has. He'll then add 80g of MgSO4, then add a lot of acetone. Then he'll just filter. Potential problems: swim remembers that this kind of solution was particularly hard to filter without a vacuum and junk, or maybe that's just because swim had to filter all this plant matter too when he did it the last time around. That, and once again, maybe the MgSO4-Na2CO3 will take a very long time to settle before swim can siphon off the acetone.
 
Well, too late...swim's on a time schedule and acted.

He weighed out 80 grams of MgSO4. Added it to a 500ml jar with some residual Xylene and Fumarate crystals. He then added the basic solution in the test tube. He used acetone to wash anything left in the test tube (turns out that clump at the bottom was in fact sodium carbonate...acetone wouldn't wash it..and water dissolved it in two seconds...swim discarded that water figuring that the acetone would have gotten rid of all the alkaloids left in the test tube.

The MgSO4 then fused into one giant clump. SWIM then added acetone, and it stayed like that. He added around 300ml of acetone.

Remembering a thread about how to make anhydrous acetone.....swim then began to shake the jar vigorously. The clumps broke up, and believe it or not, the MgSO4/Na2CO3 settled in less than 20 seconds. SWIM then shook vigorously again. Same result. The acetone took on a very slight off-white color (praying that that's freebase). He's thinking he should take a tiny sample and add FASA to see if there are in fact crystals in it.

But yeah, the stuff settled like nobody's business, this should be very easy to filter. And if this is the case, this method isn't too shabby (granted that it's the same as the method of making fumarate and Na2CO3 paste and extracting with acetone.....it just uses more water and another ingredient).

swiWE'LL see how it goes, hopefully there are crystals.

E.C.


EDIT: SUCCESS!!! SWIM took a sample (about a ml). Added about a ml of FASA...and swim's favorite needle-like crystals appeared. SWIM then just tossed this back in with the bunch. SWIM then shook up the 500ml jar vigorously. The solids in there sound like sand! But they're breaking up more...in other words, it's taking longer to settle. Nonetheless, the solids are pretty large, swim doesn't think filtering will be too bad. Coffee filter might even be just fine, but since the stuff settles so well, he'll just go ahead and use the 8um.

Thanks for the help guys.
 
Hmmm, despite the success of the crystalizing earlier....SWIM did two pulls of acetone. Then filtered using a hot water bath and fan. There was residual water left over and it's now in the oven, but it honestly does not look like the gram of fumarate swim put in (swim doubts that it's even a quarter of a gram...kind of curious what happened). Maybe swim will add a huge amount of sodium carbonate to the leftover solids, then add acetone again later....it's possible that he didn't add enough sodium carbonate in the first place (4 times the amount of fumarate?).

It's at 125F, it's going to be probably a few more hours for the water to dry, it's painfully slow.

If this doesn't turn out well, swim will probably have to cut into his 1 gram stash of fumarate and freebase it the right way....ugh. So sad.

E.C.

EDIT: oops, just kidding. So apparently when in the oven at 110 (swim reduced it to that). Everything is melted still. This morning after being left in the oven air, there are crystals everywhere, pretty dark actually, they look far from pure but swim has a very strong feeling that it's the J. Spice. The yield looks much higher now, but we'll see.

BTW, swim then took 300mg of fumarate and freebased it the right way....yes, that process is way easier haha.
 
Final yield: .540g freebase. He put in 1.2g of fumarate, so that's pretty low, but swim only did two acetone pulls rather than 4-5, that plus residual alkalkoids left in the dish from scraping...it's not bad. It's an orange/brown color, a little sticky. There were still undried oils on the dish, swim thought it was still water, but after a considerable amount of time, it refused to go away. It didn't pose any problem when scraping though, it must have just blended in. It also has that strong dmt odor.

SWIM will test out 15mg tonight (30 if that's too weak). He's never had a combination of the j.spice, oxides, and dmt before so this should be interesting. (He's only had dmt that came from a naphtha freeze...so just dmt swim assumes).

Want to thank everyone again for the help (including for the whole FASA extraction).

E.C.

EDIT: 30mg was a good dose for swim. It wasn't overwhelming and dissociating, but strong.
 
could it be that swim is not baking his bicarb long enough - it was baked at 200 celcius for 2 hours - it looked and felt different >?
 
SWIM also has been having issues with freebasing bufotenine fumarate..not sure where its all going

hes tried sodium carbonate and calcium hydroxide..and he just doesnt seem to be getting what he should
 
Phlux- said:
could it be that swim is not baking his bicarb long enough - it was baked at 200 celcius for 2 hours - it looked and felt different >?
Did SWIY weight it out before and after baking? it should be around 30% lighter (cant' remember the exact number, but that's around this value) when the conversion to carbonate is full. One can use a pH meter to verify that, sodium carbonate should give one a pH of at least (or around) 12.

SWIM's FOAF never really had problems with that. Does SWIY always weigh out the fumarates before freebasing? Does he (or she) wash the fumarates with acetone so that to eliminate any possible residual fumaric acid (should not be the case but you never know...)?

Jorkest said:
SWIM also has been having issues with freebasing bufotenine fumarate..not sure where its all going

hes tried sodium carbonate and calcium hydroxide..and he just doesnt seem to be getting what he should
SWIM's FOAF has never tried that, could it be possible that the conditions used in the bufo-fumarate to bufo FB conversion may somehow damage the bufotenin?

We know that bufotenin can withstand pH as high as 12 and a very similar method is used for bufo extraction from the seeds (watery paste w/crushed seeds + equal amount of Ca(OH)2 or Na2CO3). Should we start considering that calcium bufotenate (in case of Ca(OH)2) or sodium bufotenate (in case of Na2CO3) forms and this is insoluble in acetone?

I do not think so but who knows?
 
that shouldnt be the case because its coming out of the seeds fine..its just getting the fumarate to drop off that hasnt been working..perhaps hes not using enough? SWIM doesnt know..hes gonna continue pulling from this stuff and see what he can come up with

if this doesnt work..hes gonna stick to freebasing seeds..pull with acetone or MEK..and then just evaporating it down..and then doing the MEK:heptane mix to purify
 
swim measured the ph of his carbonate and its between 11.5 and 12 - should be fine - perhaps its the water.
 
When swim made his Sodium Carbonate...he made it at the same time he made his Anhydrous MgSO4, at 500F for over 3 hours.

SWIM's also still working on his other fumarate-to-freebase trial. This time he used calcium hydroxide and now MgSO4, he'll also probably do 4 pulls instead of just 2. Hopefully the yield should be closer to the theoretical.

E.C.
 
SWIM also has heard many reports of small yields upon converting the isolated fumerate salts to freebase. TLC results show that the product has a significant fraction of residual fumeric acid present, even after several excessive acetone washes. Additionaly the jungle spice alkaloids do not seem to be present in the freebased isolated product. Thus the isolated product is somewhat impure explaining why people are not getting the theoretical amounts of freebase even when using strong bases like KOH and NaOH. SWIM would like to see a yield comparision of isolated freebase between A/B extract, STB and FASA using same plant source. While FASA is very useful seconds looks are needed as many are reporting low yields of the freebase alkaloids. It appears a significant portion of the isolated product is sadly residual fumeric acid. This is a great technique as has immense potential but needs to be looked into deeper.

TLC shows however that the major product is DMT fumerate but the acid is never the less present. Another alkaloid may be present although it is hard to say as of yet the method needs to be tinkered with.
 
The utility of FASA however may be with plants with high fat content like cacti and phalaris and others which are hard to extract by conventional methods. But SWIM thinks the standard methods for MHRB may prove to be the most efficient. They may be similaur though in which case availability of supplies will be more important than a couple mgs.
 
okay so if swim does a naptha pull off stb then converts to fumarate then back to freebase is there a loss - swim has only done a xylene pull, fasa'd that then converted. when freebasing this there are 2 parts the jungle and the spice a naptha wash proves this.
So what should happen here - only do fasa on plants high in oils etc ?
evap ur xylene instead of fasa'ing it then freebasing ?
 
But aside from fumaric acid contamination, which isn't really that bad considering it is used to make sour candies sour, are you actually losing DMT somewhere along the process?

What I mean is, when you add for example DMT freebase to acetone, then add FASA to precipitate, are you actually losing DMT somewhere? In other words your product may be watered down, but wouldn't it still contain the same amount of DMT as before?

Because I read that the solubility of DMT fumarate in acetone is practically nil, which would mean (I assume) that if there was enough fumaric acid to completely react with all the DMT freebase, no DMT should be left in solution after the precipitate has been filtered off.
 
swims experience with smoked fumarate to freebase then spice separated with naptha was very different to normal stb naptha pulls. very different, almost like a different substance. dunno why. swim will try it again soon. There was no buzz - no colored strings in the chrysanthemum pattern, just a total shift in perception. read the most intense experience of my life in experiences area.
 
prey said:
Because I read that the solubility of DMT fumarate in acetone is practically nil, which would mean (I assume) that if there was enough fumaric acid to completely react with all the DMT freebase, no DMT should be left in solution after the precipitate has been filtered off.
Exactly.
 
Phlux- said:
swims experience with smoked fumarate to freebase then spice separated with naptha was very different to normal stb naptha pulls. very different, almost like a different substance. dunno why. swim will try it again soon. There was no buzz - no colored strings in the chrysanthemum pattern, just a total shift in perception. read the most intense experience of my life in experiences area.
Very interesting. It is hard to say whether SWIM's FOAF has noted some differences between FASA extracted spice and standard naphtha-extracted spice. But there may be actual qualitative differences, but it is difficult to say at the moment without more people reporting back.

On the other hand, spice can be totally unpredictable. When SWIM's FOAF started smoking spice, after the 4-5th time he established what he called "standard" spice experience. But the more he used it, more qualities came to the surface. From totally weird experiences to failed breakthroughs to radical shifts in consciousless to creatures literally jumping in front of his open eyes and trying to grab his pipe!

So he does not believe that there is too much of a standard experience. Maybe SWIY should smoke more of this FASA batch??
 
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