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Bufotenine Extraction Options
 
Ethnochemist
#301 Posted : 2/26/2009 6:14:57 AM

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Ah swim sees now.

Any particular recommendations for the solvent to use for "exclusive extraction" after freebasing?

E.C.
 

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69ron
#302 Posted : 2/26/2009 6:22:52 AM

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Yes. Use pure room temperature heptane, d-limonene, or xylene. But don't throw it out. They will not extract freebase bufotenine but will extract some interesting and active psychedelic alkaloids. It will be a very small amount, but has nice effects. Sort of DMT-like, but not exactly.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

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Ethnochemist
#303 Posted : 2/26/2009 6:28:19 AM

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Interesting. SWIM will definitely give that a try.

Well this sounds like an excellent TEK, certainly less complicated and less prone to error/yield loss than the last tek swim performed.

SWIM will try this out on an ounce of seeds in the near future, hopefully he can get at least 250mg of product.

Thanks for all the help and info.

E.C.
 
memo
#304 Posted : 2/26/2009 6:15:41 PM

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69Ron, your defat explanation is a jewel of insights and should be incorporated into the DMT Handbook. Thanks so much!!!!
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burnt
#305 Posted : 2/28/2009 7:19:35 PM

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SWIMs friend had a dream the other night and I thought I would relay it to you all:

After doing Ott 2001 one method to extract bufo from cebil seeds SWIMs friend decided to do a purity check on an imaginary GC-MS instrument. Note that after evaporating the non-polar (chloroform extract) a brown gooey foam formed (foam is because it was evaporated under vacuum). This was extracted a few times with mek:heptane and evaporated. It evaporated into a yellowish goo. Note that it was not recrystallized just evaporated and analyzed. Purity is really high! Almost only bufo! Nice to know sorry SWIMs friend doesn't want to post the chromatogram as this is all in his head. Also SWIMs friend is thinking about analyzing the original brown gooey to try and ID the toxins, another dream..

Now SWIMs friend has some questions about recrystallization as its been a bit problematic with this compound. Ethyl acetate isn't working well even if solvent is cooled warmed cooled warmed cooled warmed, the crystals never really make it.

Has anyone noticed anything about MEK and stability? SWIMs friend found some laying around and it had a slight yellow tint!? That doesn't seem normal. Anyway SWIMs friend ran out of the stuff and is seeking substitutes.

Anyway can acetone replace MEK for this kind of recrystallization? SWIM doesn't see too many reasons why it couldn't as long as its anhydrous. SWIMs friend still has a lot of that brown gooey foam and wants to clean it up and get some xstals.
 
69ron
#306 Posted : 2/28/2009 8:17:06 PM

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Sounds like the MEK is messed up. It should have produced crystals from Ott’s tech. SWIM knows because he tried it and got really clean crystals from it by starting with Ott’s tech. MEK should be completely clear, not colored at all.

Acetone can be used instead, but the ratio of acetone:heptane is unknown. Acetone is a little more polar than MEK so the 2:3 ratio of MEK:heptane will be too polar if you substitute acetone for MEK. You'll need to either reduce the acetone a little or add a little more heptane.

Note that if there’s any fat or oil present (there’s a lot of fat and oil in the seeds) the bufotenine might not crystallize. When doing an A/B on the seeds you need to defat at least 5-10 times.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
memo
#307 Posted : 2/28/2009 8:26:42 PM

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SWIM has a brownish hardened goo left after evaporating MEK/Heptane following the same TEK and with similar results that Ethnochemist did. It may be about 200mg left from 114gr of Cebil seeds. Rinsed the goo with heptane and naphtha for good measure. Was wondering if there is a good way to get this to crystallize. Thought about redissolving in MEK/Heptane and letting the MEK vap off thinking that the Bufo would crystallize out into the remaining Heptane but seeing that Heptane is more volatile than MEK he doesn't think that this would be a good idea. SWIM believes he's at about the same point that burnt's SWIM's friend is at. SWIM was considering redoing an A/B to clean it up some more.
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burnt
#308 Posted : 2/28/2009 8:40:18 PM

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Yea SWIMs friend got weirded out by the color of the MEK and decided not mess with it anymore (its an old bottle). SWIM defatted at least 6 times with CHCl3 (100mL per pull) against acidic water. Doesn't seem like it was enough as there was a lot of brown oily material + a whitish foam after doing the CHCl3 pulls against pH 9.5 H2O. Oil amounts can vary and SWIMs friend worked quickly during these pulls so its not a big surprise.

Perhaps 1:4 acetone may work. Perhaps A/B redo would be best option SWIMs friend thinks its the oils. Will report after a few more lucid dreams. Its always fun figuring out a diff compound.
 
Ethnochemist
#309 Posted : 3/1/2009 1:12:05 AM

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Yeah, swim still isn't sure what to do with his 150mg or so bufo....it doesn't seem to be getting any cleaner with the MEK:Heptane washes. The MEK does in fact evaporate first leaving behind crystals in the heptane. There's just too little of them to actually pour off the heptane.

SWIM is also in the process of his 25g seed extraction. He defatted about 5 times with MEK first, then twice with heptane. SWIM didn't do a thorough defat, the solvent was still a little yellow, but swim couldn't completely tell since he didn't let the particles completely settle each time. Then he freebased using sodium carbonate. SWIM then did two heptane washes....the heptane is very yellow, swim stopped after two since he was running out of heptane (he still needs more for the MEK:Heptane pull).

Right now he is in the process of pulling with MEK:Heptane, waiting for the particles to settle enough so that it will gravity-filter at a decent pace.

The MEK:Heptane, after letting the particles settle, will probably be yellow. If that's the case, swim will evap the the MEK:heptane (praying for crystals to appear), and then try to separate the dirty heptane from them...possibly wash them. And hopefully swim will have enough MEK:Heptane to maybe wash it again.

E.C.

EDIT: SWIM only has 250ml left of MEK:Heptane Sad The MEK:Heptane extraction is in fact piss yellow color..evaporating now...The solvent is cloudy...but swim can't really estimate anything until most of it has evaporated.

EDIT2: Crystals! SWIM will get the yield in a little bit. But at least this time they are the same color as the MEK:Heptane...a yellow color, rather than brown like swim's last stuff. SWIM will taste this stuff first...if it's too harsh..swim will wash the rest. Yay! SWIM likes this method so far...he's got results and the procedure was much shorter.

EDIT3: 650mg!! And it's way purer than swim's other bufotenine which was washed 4 times with MEK:Heptane!!! SWIM got a yield 4 times as high....and used 4 times less material. At least swim knows which tek he'll be using from now on.....yeesh.

It's kind of an orangish color (like those pictures of dmt on erowid)...he'll do some MEK:Heptane washes using the minimum required amount of MEK:Heptane.

EDIT4 (Last for the night): It's now sitting in a test tube in approx. 50ml of MEK:Heptane. Red, disgusting goo sitting at the bottom, but the MEK:Heptane itself is still a piss yellow...which means the final product will also be not so pure. Either way, swim's looking at this stuff compared to his other bufo....maybe this stuff will at least be smokeable.
 
Ethnochemist
#310 Posted : 3/2/2009 9:08:00 PM

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Well, swim can't purify this junk any further. SWIM's first MEK:Heptane wash resulted in DIRTIER CRYSTALS!!! They looked exactly like DMT+J. Spice. SWIM then wanted to try a Xylene boil. Instead, he found that the Xylene was very dirty, so he washed his extract twice with Xylene (it was clear after that). He then did another MEK:Heptane wash (which left behind a tremendous amount of red goo), and his crystals are now a light orange.

SWIM will just try to smoke this stuff as it is and hope for the best.

In the future, swim will definitely be more thorough with the defats. He'll defat with Xylene, then MEK, and Heptane until they all turn out clear. Then he'll do the same after freebasing. This will probably take much longer, but it should yield some VERY clean results.



E.C.
 
Ethnochemist
#311 Posted : 3/3/2009 7:52:13 AM

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Grrr, no luck once again. SWIM vaped 15mg over the course of 4 min in small hits, this time he could hold it in. The first hit made his arms feel sore like always...then it hit his head. But swim feels just like last time, except weaker (maybe because there are less toxins). Only the usual very mild visuals.

SWIM's really not having any luck with this stuff. Maybe he has to take large hits for it to work. But he can't hold those in anyway.

SWIM will probably just stick to snuff (snuff works for him, but hates the side effects..and it's hard to make it right), unless he can do something else with this stuff. Seems painful to snort (or useless?)...what about sublingual?

E.C.
 
burnt
#312 Posted : 3/3/2009 8:50:09 AM

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SWIM had another lucid dream last night and thought SWIM would relay to you all:

Redid acid base extraction on 1.2g of bufo + small amount of brown goo. After dissolving the material in acidic water defat 3x with chloroform and 3x with hexane. Rebasified with ammonium hydroxide and reextract 9x with chloroform. The different in material was only 10mg. Either way the stuff still won't recrystallize easily from ethyl acetate.

So after getting back the whiteish foam + brown goo ---> SWIM tried acetone : heptane 1:4 and some (20mg or so) pinkish crystals were squeezed out after evaporating acetone. SWIM needs to play with the ratios a bit and try to perfect this. Possibly some other solvents, heat, etc.

Then SWIM woke up from that interesting dream.

Ethno maybe SWIY should try to redo the A/B. Its a lot more work but it might do the trick in getting out that gooey material. SWIM will try and continue to have lucid dreams to see if this stuff can be cleaned any other ways.

Edit: Wow SWIM is getting good at lucid dreaming. Anyway in the last dream SWIM decided that acetone : heptane while it can work doesn't work so nice. SWIM went back to ethyl acetate and is dreaming of much better results. It takes time and patience to crystallize with that solvent but the stuff looks much cleaner.
 
Fatcat
#313 Posted : 3/9/2009 6:04:01 PM

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If no one is already working towards a D-Limonene precip, I will order some seeds now and start gathering some materials. Just out of curiosity, if it doesn't work, what would be the easiest way to clean to pureish without MEK Heptine?

I will try to follow your instructions the best I can with my limited knowledge of chemistry (I do know a decent amount of physics). It would take me a few weeks to un-suspiciously gather all the materials to make it because there is only one Ace around here that has everything I need. And I know I can get D-limonene from a local home depot.

I am extremely interested in bufotenin, I plan on doing extensive (amateur) studies on the types of visions tryptamines produce, and if I am clear minded I can take observations much more accurately.

Will post more when I start.
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Jorkest
#314 Posted : 3/9/2009 11:20:00 PM

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SWIM is just waiting for his d-limonene..and once he has it..he will be working on the purifying stage
it's a sound
 
Dorge
#315 Posted : 3/10/2009 10:41:46 PM

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Ok so swim is some what of a NooB when it comes to extractions and chemistry so bear with him...

Swim Has produced a fairly successful batch of red Resin From the Acetone calcium hydroxide Tek found on Erowid. THe results from vaporizing the resin is very slight CLosed eye visuals... moving basic colored wires and shapes on a dark screen... not much... but more then smoking seeds alone.
Swim was one of the first to write about Edible limes addition to Seeds for snuffing. Swim is used to very powerful visions from snuff and knows this plants effects like the back of Swims clammy little hand... so Swim feels the resin is definitely subpar...
SO...
what Swim is wondering and asking your bright SWIYs is how might one take this resin and turn it into THe lovely crystals with the no body load and clear visions that 69ron has spoken off?
SWIMS not sure how to get ahold of MEK in the USA ( if any one has any ideas PM SWim)So swim is wondering if swim could work with naphtha to further purify it down. Swim read that it was mentioned as a possible alternative to MEK and Heptane mix... so Swim is curious if its been tried and How Swim might attempt it with Naphtha.
any help would be wonderful...
Pax

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memo
#316 Posted : 3/10/2009 11:45:19 PM

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MEK is available at large chain hardware stores in the paint thinner/solvents area. I'm afraid that unless you did a lot of initial defatting that you may end up with nothing when trying to reduce it down to crystals. If you read back in this thread there are a couple of people that had this problem and I believe it is because oils were not initially washed out well enough to get crystals to form. It seems that a lot of people lose a lot of product in the process of doing A/B transitions or there is some oil that will happily transition between a salt and a freebase form and follow the target alkaloid if you don't get it out early enough.
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Dorge
#317 Posted : 3/11/2009 1:19:44 AM

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Ok... thanks.
So has there been any successful repeats of this method with MEK? and Bioassys that are similar to the results that SwIy has spoken of? ive ogne through most of this post and I have not seen many results as of yet.
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Jorkest
#318 Posted : 3/11/2009 1:43:15 AM

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SWIM has gotten crystals...but only been able to produce visions a few random times..most other times..have been subpar..perhaps this is because of smoking method..but it HAS worked..just not consistently
it's a sound
 
Dorge
#319 Posted : 3/11/2009 2:48:05 AM

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what does one make of that?
why is this tek so hard to repeat? bioassy as well?
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Jorkest
#320 Posted : 3/13/2009 2:49:09 AM

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Quote:

Infundibulum wrote:
69ron wrote:
SWIM is wondering if hot d-limonene (160 C) could melt and dissolve bufotenine. D-limonene boils at 176 C which is plenty hot enough to melt bufotenine but not hot enough vaporize it away. At 160 C, all the freebase bufotenine would be melted making it soluble in solvents it's normally insoluble in. Just like with xylene where its insoluble in room temperature xylene but soluble in boiling xylene, maybe the same would be true for d-limonene. If d-limonene could be used instead, you'd have a much healthier product. D-limonene is non-toxic and easily found in food grade form. If the bufotenine can be melting and dissolved in hot d-limonene and then cooled and crystallized in it, you'd pour off the d-limonene and leave behind the cystals. Even if a tiny bit of d-limonene was left behind, it would be non-toxic and smell and taste like oranges at worst.

Has anyone given d-limonene a try yet?

Not necessarily re to the highlighted point. Melted dmt-n-oxide will not mix with hot or cold naphtha. And melted naphtha will not mix with melted water!

But it would be really lovely to find out. limonone however has a much higher partition coefficient than xylene (3.7 compared to 2.9) so it would be more difficult to dissolve bufotenine.

Of course, nothing is better that trying itVery happy


Keep in mind that solubility cannot be accurately predicted by any means known to man as of yet. All methods of predicting solubliity are inaccurate for many compounds. For example DMSO can dissolve many compounds it should not dissolve according to it's XLogP.

I know the XLogP of d-limonene is higher than xylene. But it's not as high as heptane.
Bufotenine is very slightly soluble in boiling heptane. But boiling heptane won't bring bufotenine to it's melting point thereby increasing it's solubility, but d-limonene will. It doesn't much matter if it becomes soluble. What matters is that it melts and doesn't sink like the impurities do. A suspension is good enough to get it to work.

Anyway enough useless talk. SWIM will test it and see what reality has to say about it. That's the only way of really knowing.


SWIM will be trying the boiling d-limonene trick with some bufotenine..

that is unless somebody has done it and failed.....
it's a sound
 
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