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Bufotenine Extraction
- Thread starter acolon_5
- Start date
SpasticSpaz
Rising Star
So right now the all the procedures proposed have too many steps for me. (I'm a big fan of how short and simple an STB->Freeze precip DMT tek is and how good the results are for that).
Would the following tek work to give me near pure bufo?
1. Powder colubrina
2. Defat extensively with warm heptane
3. Freebase with sodium carbonate
4. Dry with MgSO4
5. Extract with MEK:Heptane
6. Boil down MEK:H till cloudy
7. Let sit overnight
Would the following tek work to give me near pure bufo?
1. Powder colubrina
2. Defat extensively with warm heptane
3. Freebase with sodium carbonate
4. Dry with MgSO4
5. Extract with MEK:Heptane
6. Boil down MEK:H till cloudy
7. Let sit overnight
Ethnochemist
Rising Star
69ron said:
Any pics of the results from this, or yield data? Earlier in the thread swim believes someone mentioned that the crystals are whitish-yellow (indicating that someone successfully tried this?). Another swimmer got black stuff
SWIM was just wondering if sodium carbonate was a strong enough base for the job, if so, how much? SWIM also read that ammonia could work (10% ammonium hydroxide solution okay? how much?)
Other questions: Coffee filters should work okay?...and...no hotplate, but what about electric stove under cooking hood? (it's essentially the same thing, no?
Thanks! SWIM's in love with this method.
E.C.
SWIM went on vacation for a bit..so hes slowly sinking back into his dreams of bufo extraction..
for the longest time he was having major issues with getting his freebase bufo to come out using calcium hydroxide...and he learned from 69ron that calcium hydroxide takes a long time to freebase things AND it doesnt stay at the desired pH..so sodium carbonate is going to be used from now on...easy as hell to get or make..
so the problem with defatting with boiling xylene is that it REALLY stinks..and its dangerous..that is a lot of fumes...so SWIM has been thinking...
1. grind seeds and then lightly toast them (he thinks this will toast out more of the junk)
2. freebase with sodium carbonate and some water, mix for 10 minutes and then let it dry (SWIM likes to let this stuff dry on its own with just a little bit of heat..rather than using another chemical like baked epsom salt)
3. extract with acetone and then filter out solids (SWIM finds it best to let the acetone sit for awhile so that any other particles settle and kinda stick to the bottom of the jar)
4. now you could evaporate the acetone for a bunch of gunk..probably be sticky and not so pretty you could then defat this with room temp xylene(SWIM feels like this might work better than defatting straight from the seeds because of a smaller amount of material)
5. then after the defat with cool xylene...add fresh xylene to the mix and boil for 5 minutes and then pour out hot xylene into cooling jar
6. once the xylene cools there should be some nice clean looking bufo crystals..pour out xylene and scrape crystals out of the jar and spread them over a flat piece of glass...really work the crystals over the glass(this should help break up the crystalline structure...thus releasing any excess xylene possibly caught in the crystals)
7. you could then wash them with heptane if you wanted..to clear out any other xylene residue(heptane evaps much cleaner)
now...at number four you could instead of evaping the acetone you could drop out the bufocrud with FASA or citric acid saturate acetone..collect the bufo fumarate or citrate and then freebase it again with sodium carbonate
5b. the FASA should defat the concoction..and you will be left with bufo + other crap you dont want...so once you freebase with sodium carbonate and some water..let it dry..however you please...and then pull again with acetone
6b. you will only need to use about between 100-200ml of acetone to get most(this hasnt been tried in his dreams yet) evaporate the acetone down for defatted bufo plus gunk you dont want
7b. you can then do the MEK:heptane mix or you can do the boiling xylene trick
granted its not as easy as 69rons four step process..but you will be using MUCH less xylene(which SWIM hates) or you dont have to use it at all...boiling xylene is gross..it stinks really bad..and the fumes are dangerous..so if SWIY can get away with using between 100-200ml of xylene to get pure crystals..instead of a few liters(because of defatting with xylene...it takes a LOT)..SWIM feels it would be worth it
for the longest time he was having major issues with getting his freebase bufo to come out using calcium hydroxide...and he learned from 69ron that calcium hydroxide takes a long time to freebase things AND it doesnt stay at the desired pH..so sodium carbonate is going to be used from now on...easy as hell to get or make..
so the problem with defatting with boiling xylene is that it REALLY stinks..and its dangerous..that is a lot of fumes...so SWIM has been thinking...
1. grind seeds and then lightly toast them (he thinks this will toast out more of the junk)
2. freebase with sodium carbonate and some water, mix for 10 minutes and then let it dry (SWIM likes to let this stuff dry on its own with just a little bit of heat..rather than using another chemical like baked epsom salt)
3. extract with acetone and then filter out solids (SWIM finds it best to let the acetone sit for awhile so that any other particles settle and kinda stick to the bottom of the jar)
4. now you could evaporate the acetone for a bunch of gunk..probably be sticky and not so pretty you could then defat this with room temp xylene(SWIM feels like this might work better than defatting straight from the seeds because of a smaller amount of material)
5. then after the defat with cool xylene...add fresh xylene to the mix and boil for 5 minutes and then pour out hot xylene into cooling jar
6. once the xylene cools there should be some nice clean looking bufo crystals..pour out xylene and scrape crystals out of the jar and spread them over a flat piece of glass...really work the crystals over the glass(this should help break up the crystalline structure...thus releasing any excess xylene possibly caught in the crystals)
7. you could then wash them with heptane if you wanted..to clear out any other xylene residue(heptane evaps much cleaner)
now...at number four you could instead of evaping the acetone you could drop out the bufocrud with FASA or citric acid saturate acetone..collect the bufo fumarate or citrate and then freebase it again with sodium carbonate
5b. the FASA should defat the concoction..and you will be left with bufo + other crap you dont want...so once you freebase with sodium carbonate and some water..let it dry..however you please...and then pull again with acetone
6b. you will only need to use about between 100-200ml of acetone to get most(this hasnt been tried in his dreams yet) evaporate the acetone down for defatted bufo plus gunk you dont want
7b. you can then do the MEK:heptane mix or you can do the boiling xylene trick
granted its not as easy as 69rons four step process..but you will be using MUCH less xylene(which SWIM hates) or you dont have to use it at all...boiling xylene is gross..it stinks really bad..and the fumes are dangerous..so if SWIY can get away with using between 100-200ml of xylene to get pure crystals..instead of a few liters(because of defatting with xylene...it takes a LOT)..SWIM feels it would be worth it
Ethnochemist
Rising Star
Approximately how much Sodium Carbonate (relative to seeds) would swiy say would be good?
Couldn't swiy just wash the fumarates with acetone until they're pretty and white? Or will they turn brown again upon freebasing? or will those impurities come out with the Xylene boil anyway?
The defat-shortcut is nice Wouldn't pulling it again with acetone pull the "other crap" with it as well? SWIM doesn't understand. The stuff (like N-oxides) that came with the Fumarates would just freebase again, no?
And after the final pull of acetone (and then that acetone's evaporation), the crystals will be amber-brown? (according to the citric acid procedure). And then the Xylene-boiling step will be much whiter?
SWIM would also like a little advice on that step. How easy is it to pour off boiling Xylene (bubbles and all) without disturbing the tiny impurity particles on the bottom? (if they're even on the bottom cus of the bubbles)
Really appreciate this..
E.C.
Couldn't swiy just wash the fumarates with acetone until they're pretty and white? Or will they turn brown again upon freebasing? or will those impurities come out with the Xylene boil anyway?
Jorkest said:
The defat-shortcut is nice
Wouldn't pulling it again with acetone pull the "other crap" with it as well? SWIM doesn't understand. The stuff (like N-oxides) that came with the Fumarates would just freebase again, no?And after the final pull of acetone (and then that acetone's evaporation), the crystals will be amber-brown? (according to the citric acid procedure). And then the Xylene-boiling step will be much whiter?
SWIM would also like a little advice on that step. How easy is it to pour off boiling Xylene (bubbles and all) without disturbing the tiny impurity particles on the bottom? (if they're even on the bottom cus of the bubbles)
Really appreciate this..
E.C.
SWIM usually uses equal parts..just to make sure..but half the amount of the seeds SHOULD do it..
and what happens with the FASA is that you are dropping everything out of the acetone BUT the fats..so you are getting bufotenine plus all the other crap that is in there..so the first acetone pull followed by the FASA is the defatting step ONLY...you then have to freebase that again...
you could just go to the xylene boil from this stage..
so here
1. grind seeds and toast
2. freebase with sodium carbonate and water to form a paste...then let it dry
3. pull with acetone and then filter out solids
4. add FASA to bufo acetone..to drop bufo fumarate..plus other crap
those four steps are JUST for defatting
5. freebase bufocrap fumarate with sodium carbonate and water to form a paste...let this dry completely
6. pull with acetone and evaporate(this will seperate the any excess sodium carbonate and other solid left overs)
7. boil what came out of the acetone pull with xylene for 5 minutes OR use MEK:heptane combo
those three steps are to separate the bufotenine from the other nauseating substances and any random solids that are present
8a. if xylene boil was done..pour boil xylene into new jar and let it cool
8b. if MEK:heptane was used..pour mixture into clean jar and let it evaporate..you can use heat if you want..you can even boil it off..but the slower the evaporation..the bigger the crystals..THESE CRYSTALS ARE READY TO SMOKE
9. once xylene sits for say a day..pour it off..and scrape crystals off inside of jar..wash these with heptane(removes residual xylene) and then let crystals dry..THESE ARE READY TO SMOKE
you can always rextalize with MEK:heptane after the xylene boil to get bigger crystals...
and to answer you last question..about the xylene boil...most of the solids stay on the bottom..like a tar...or oil..
and what happens with the FASA is that you are dropping everything out of the acetone BUT the fats..so you are getting bufotenine plus all the other crap that is in there..so the first acetone pull followed by the FASA is the defatting step ONLY...you then have to freebase that again...
you could just go to the xylene boil from this stage..
so here
1. grind seeds and toast
2. freebase with sodium carbonate and water to form a paste...then let it dry
3. pull with acetone and then filter out solids
4. add FASA to bufo acetone..to drop bufo fumarate..plus other crap
those four steps are JUST for defatting
5. freebase bufocrap fumarate with sodium carbonate and water to form a paste...let this dry completely
6. pull with acetone and evaporate(this will seperate the any excess sodium carbonate and other solid left overs)
7. boil what came out of the acetone pull with xylene for 5 minutes OR use MEK:heptane combo
those three steps are to separate the bufotenine from the other nauseating substances and any random solids that are present
8a. if xylene boil was done..pour boil xylene into new jar and let it cool
8b. if MEK:heptane was used..pour mixture into clean jar and let it evaporate..you can use heat if you want..you can even boil it off..but the slower the evaporation..the bigger the crystals..THESE CRYSTALS ARE READY TO SMOKE
9. once xylene sits for say a day..pour it off..and scrape crystals off inside of jar..wash these with heptane(removes residual xylene) and then let crystals dry..THESE ARE READY TO SMOKE
you can always rextalize with MEK:heptane after the xylene boil to get bigger crystals...
and to answer you last question..about the xylene boil...most of the solids stay on the bottom..like a tar...or oil..
Ethnochemist said:The defat-shortcut is nice
SWIM believes this to be referring to some of the more toxic alkaloids found in the seeds, as most seeds seem to be somewhat toxic.
amor_fati said:Ethnochemist said:The defat-shortcut is nice
SWIM believes this to be referring to some of the more toxic alkaloids found in the seeds, as most seeds seem to be somewhat toxic.
yes this would pull the 'other crap' as well..but the FASA is only to remove fats and oils from the mix..not to remove any of the toxic alkaloids..
so far the only ways that we know of(thanks to 69ron) to easily separate the toxic chemicals from the bufo is either the MEK:heptane mix or the xylene boil
Ethnochemist
Rising Star
Ah okay, swim sees now. Makes sense. Great info!
A few more questions...
Heptane availability? SWIM remembers seeing MEK at the hardware store....never seen heptane though. Maybe his local science shop has it? Or is there an easier source?
What was the ideal MEK:heptane mix? 40:60?
Ugh, Xylene, swim may even turn the Xylene+Crystals back into fumarate, just so he can wash off the xylene with acetone (If he can't get heptane).
And lastly....SWIM's really starting to like the ammonia idea. 10% ammonia (janitorial strength) to use for freebasing. It smells bad, but it's safe and doesn't introduce another ingredient. SWIY can just add enough ammonia to the seeds to make them pasty (if they even become pasty)....better coverage so mixing shouldn't be as much of an issue. And then swiy can just put it in the oven at 250 to evaporate the water/ammonia. SWIM thinks that this would also make pulling from the seeds with acetone easier, since sodium carbonate particles are tiny and clog the filter well.
Another note, swim would skip the drying step after FASA. Why not just wash with acetone maybe 3 times, then add base + water (or ammonia!), and then directly to that, pull with MEK:heptane a few times? Everything bad should stay in the water, right? The only thing acetone really leaves behind is the sodium carbonate anyway. Just a thought.
E.C.
A few more questions
...Heptane availability? SWIM remembers seeing MEK at the hardware store....never seen heptane though. Maybe his local science shop has it? Or is there an easier source?
What was the ideal MEK:heptane mix? 40:60?
Ugh, Xylene, swim may even turn the Xylene+Crystals back into fumarate, just so he can wash off the xylene with acetone (If he can't get heptane).
And lastly....SWIM's really starting to like the ammonia idea. 10% ammonia (janitorial strength) to use for freebasing. It smells bad, but it's safe and doesn't introduce another ingredient. SWIY can just add enough ammonia to the seeds to make them pasty (if they even become pasty)....better coverage so mixing shouldn't be as much of an issue. And then swiy can just put it in the oven at 250 to evaporate the water/ammonia. SWIM thinks that this would also make pulling from the seeds with acetone easier, since sodium carbonate particles are tiny and clog the filter well.
Another note, swim would skip the drying step after FASA. Why not just wash with acetone maybe 3 times, then add base + water (or ammonia!), and then directly to that, pull with MEK:heptane a few times? Everything bad should stay in the water, right? The only thing acetone really leaves behind is the sodium carbonate anyway. Just a thought.
E.C.
first of all...a good source of heptane is called Bestine..its a rubber cement remover you can get at art stores..like real art store..
next the MEK:heptane should be 2:3..or 40:60..but 2:3 same thing...two parts MEK three parts Heptane..
and SWIM likes the idea of using ammonia..but he cant get any good stuff easily..and is not sure how it will work..probably fine though..
and about the drying after FASA..im not sure where that came from..washing with acetone will work great..to get rid of any excess fumaric acid..and any other fats and oils that may have gotten in there...there is no need to fully evaporate after the FASA..
and about mixing the water with the MEK:heptane mix might mess up the solubility of the bufotenine because MEK mixes with water
next the MEK:heptane should be 2:3..or 40:60..but 2:3 same thing...two parts MEK three parts Heptane..
and SWIM likes the idea of using ammonia..but he cant get any good stuff easily..and is not sure how it will work..probably fine though..
and about the drying after FASA..im not sure where that came from..washing with acetone will work great..to get rid of any excess fumaric acid..and any other fats and oils that may have gotten in there...there is no need to fully evaporate after the FASA..
and about mixing the water with the MEK:heptane mix might mess up the solubility of the bufotenine because MEK mixes with water
Ethnochemist
Rising Star
Thanks for the source tip!
Oh crap...didn't know MEK and water were miscible. Okay, so then for the second freebase, swim will just use a small amount of ammonia, and dry it the same way he did with the seeds. Fumaric acid would be left over though, does fumaric acid dissolve in MEK:Heptane?
As for ammonia availability, yeah it's real easy to get over here. From Ace Hardware, Janitorial Strength (10% or so).
Great info, swim will definitely try out this TEK, probably in 2.5 weeks, maybe sooner.
This is the final write-up..
1. Dry seeds in oven at 250F for 2 hours.
2. Grind seeds (coffee grinder).
3. Place in a dish, add enough 10% ammonnia to make "soggy seeds" but try to avoid excess ammonia dripping around. Let sit for 10 min.
4. Dry in oven at 250F for (???) hours (until ammonia smell gone).
5. Pull with acetone 3 times (3-4 parts by volume per pull).
6. Evaporate acetone down to half it's original volume (hot water bath).
7. Add FASA dropwise until precipitation no longer occurs. (Can't add too much)
8. Pour off acetone.
9. Wash with acetone 3 times (SWIM will do this in a 50ml test tube), or until color stops changing.
10. Pour off last acetone and spread the goods out on a dish.
11. Add enough ammonia to make pasty. (Stuff will dissolve if it doesn't freebase). Let sit for 10 min.
12. Dry in an oven at 250F until ammonia smell is gone. (an hour maybe?)
13. Pull with MEK:Heptane-2:3
14. Evaporate the the MEK:Heptane.
15. Enjoy!
Would probably take 2-3 days. (1-2 if swiy has time and privacy).
E.C.
Oh crap...didn't know MEK and water were miscible. Okay, so then for the second freebase, swim will just use a small amount of ammonia, and dry it the same way he did with the seeds. Fumaric acid would be left over though, does fumaric acid dissolve in MEK:Heptane?
As for ammonia availability, yeah it's real easy to get over here. From Ace Hardware, Janitorial Strength (10% or so).
Great info, swim will definitely try out this TEK, probably in 2.5 weeks, maybe sooner.
This is the final write-up..
1. Dry seeds in oven at 250F for 2 hours.
2. Grind seeds (coffee grinder).
3. Place in a dish, add enough 10% ammonnia to make "soggy seeds" but try to avoid excess ammonia dripping around. Let sit for 10 min.
4. Dry in oven at 250F for (???) hours (until ammonia smell gone).
5. Pull with acetone 3 times (3-4 parts by volume per pull).
6. Evaporate acetone down to half it's original volume (hot water bath).
7. Add FASA dropwise until precipitation no longer occurs. (Can't add too much)
8. Pour off acetone.
9. Wash with acetone 3 times (SWIM will do this in a 50ml test tube), or until color stops changing.
10. Pour off last acetone and spread the goods out on a dish.
11. Add enough ammonia to make pasty. (Stuff will dissolve if it doesn't freebase). Let sit for 10 min.
12. Dry in an oven at 250F until ammonia smell is gone. (an hour maybe?)
13. Pull with MEK:Heptane-2:3
14. Evaporate the the MEK:Heptane.
15. Enjoy!
Would probably take 2-3 days. (1-2 if swiy has time and privacy).
E.C.
69ron
Rising Star
That's just an idea SWIM had...SWIM hasn't tried it himself yet.
SWIM’s actual bufotenine extractions nearly all involve using a Soxhlet with 91% IPA, and he usually does an A/B with DCM after that, so his tech’s are not normally suitable to the average kitchen chemist. The MEK:heptane and the xylene boil purification steps that SWIM developed, were all performed after a thorough A/B extraction, so his results are really pure.
At some point SWIM will get back into this and try to help develop an easy tech anyone can preform. Right now he’s working with cactus and mescaline, trying to improve his extraction skills.
SWIM’s actual bufotenine extractions nearly all involve using a Soxhlet with 91% IPA, and he usually does an A/B with DCM after that, so his tech’s are not normally suitable to the average kitchen chemist. The MEK:heptane and the xylene boil purification steps that SWIM developed, were all performed after a thorough A/B extraction, so his results are really pure.
At some point SWIM will get back into this and try to help develop an easy tech anyone can preform. Right now he’s working with cactus and mescaline, trying to improve his extraction skills.
prey..swim tried that simple extraction..and there were some issues..it took a LOT of xylene to defat it..it was gross..and SWIM was using calcium hydroxide..which SWIM has learned takes a long time to really freebase anything..and also doesnt hold its pH very well..so hes gonna stick with sodium carbonate
rellik
Rising Star
yah these beans are very fatty, SWIM is trying the 4 step tek on a small scale recently and their friend told me clearly not enough defatting was done. they told me the xylene fumes were nauseating beyond belief.
as others have mentioned using the FASA method as a defat may work better.
as others have mentioned using the FASA method as a defat may work better.
Ethnochemist
Rising Star
After defatting utilizing FASA and acetone washes......then freebasing again, would one say that only 1 purification using MEK/Heptane would be sufficient? Or would a Xylene boil + MEK/Heptane purification be necessary? (SWIM noticed Jorkest doing xylene boil and mek/heptane purification several pages back), just wondering what it'd look like without the Xylene boil.
69Ron's looked good after only the MEK/Heptane, but as he mentioned before, he did an A/B with DCM.
E.C.
69Ron's looked good after only the MEK/Heptane, but as he mentioned before, he did an A/B with DCM.
E.C.
prey
Rising Star
This may be a dumb question but...
Couldn't SWIY take the freebase crystals that precipitated from xylene, and dissolve them into acetone? The xylene should be liberated from the crystals as they dissolve in acetone, and then they would evaporate away, no?
Of course this could leave some acetone left in SWIY's crystals, but acetone is much less toxic and much more volatile than xylene.
Couldn't SWIY take the freebase crystals that precipitated from xylene, and dissolve them into acetone? The xylene should be liberated from the crystals as they dissolve in acetone, and then they would evaporate away, no?
Of course this could leave some acetone left in SWIY's crystals, but acetone is much less toxic and much more volatile than xylene.