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Soxhlet Bufotenine Extraction Options
 
ThirdEyeVision
#1 Posted : 2/19/2010 4:48:57 PM

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A friend of mine is going to do a pull on some cebil seeds using his soxhlet. His plan:
1) toast seeds.
2) grind seeds.
3) put ground seeds in beaker and ad naptha to defat. Repeat until naptha remains clear. Decant and keep solids.
4) dry seeds of naptha.
5) basify with hydrated lime and little water.
6) toast again to dry.
7) load into soxhlet and pull with DCM over night.
8 ) reduce solvent via distilation.
9) salt with diluted HCL

Does this procedure sound feasible?
Is this the best solvent/acid combo?


ThirdEyeVision
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soulfood
#2 Posted : 2/19/2010 5:09:42 PM

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I'd defat with DCM in the soxhlet. Naphtha won't get rid of anywhere near enough fats. Then I'd base and pull with IPA and evap. Then use acetone/mek:heptane/naphtha mix or xylene boil to clean up the extract.
 
OriginalFace
#3 Posted : 2/19/2010 5:16:35 PM

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Remember to snap your seeds in two before toasting or they will explode like popcorn when you put them in the oven.

And don't forget to open the window to let the nasty smell outStop

OF


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But I can't be happy,
'till I make you happy, too Pleased

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ThirdEyeVision
#4 Posted : 2/19/2010 8:58:28 PM

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Thank you for the help!
So revised plan to:

1) toast seeds, snap in half first. 
2) grind seeds.
3) Defat with DCM in soxhlet until clear.
4) dry seeds of DCM.
5) basify with hydrated lime and little water.
6) toast again to dry.
7) load into soxhlet and pull with IPA over night.
8 ) reduce solvent via distilation.
9) evap remaining IPA
10) clean with MEK/heptane mix.

That would be pulling the free base, is that a stable form for storage or just for use?
ThirdEyeVision
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ThirdEyeVision
#5 Posted : 2/19/2010 9:17:02 PM

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soulfood wrote:
I'd defat with DCM in the soxhlet. Naphtha won't get rid of anywhere near enough fats. Then I'd base and pull with IPA and evap. Then use acetone/mek:heptane/naphtha mix or xylene boil to clean up the extract.


Has anyone zeroed in on the right acetone:mek combo? I pulled up the old 69Ron thread and the heptane:naptha mix was settled but not the acetone:mek. Anyone know anyone who continued experimenting with that combo? Heptane is just so expensive.
ThirdEyeVision
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Jorkest
#6 Posted : 2/19/2010 9:59:24 PM

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you dont want to use acetone and mek..you need either acetone and heptane....acetone or naphthat...or mek and heptane or mek and naphtha
it's a sound
 
ThirdEyeVision
#7 Posted : 2/20/2010 5:55:55 AM

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Jorkest wrote:
you dont want to use acetone and mek..you need either acetone and heptane....acetone or naphthat...or mek and heptane or mek and naphtha

Thanks, I fixed it.

Soulfood, so DCM has worked best for your friends defat? I know in freebase form bufotenine is highly soluble in DCM, was there any loss in yield defatting with DCM? Obviously it is still in salt form and I guess the salt isn't soluble at all.
ThirdEyeVision
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The 8th Light, is gonna shine bright tonight
 
soulfood
#8 Posted : 2/20/2010 9:42:08 AM

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That's right.
 
D_Juggz
#9 Posted : 2/24/2010 12:53:53 PM

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Stop Stop
HELL YES! Thanks so much for this thread!
ThirdEyeVision - My friend is going to try the same thing but here is his plan: Cool

1) Toast seeds, snap in half first.
2) Grind seeds in a herb grinder untill fine
3) Put powder in soxhlet, using a cotton bud as a stopper top and bottom.
4) Run overnight with acetone 60-70ml
Quote:
69Ron: Acetone @ 20 C: soluble (5 g/100 ml)

5) Add vinigar to salt out bufotenine.
6) Pour off acetone, and let it dry out.
7) Convert the left over solids back to Bufotenine freebase by adding a spoonful(2g) of Sodium Carbonate and just enough water to turn them into a pasty consistency. Dry completely.
8 ) load into soxhlet and pull with IPA over night.
9) reduce solvent via distilation.
10) evap remaining IPA
11) Not sure how to clean it? does he need to? what other toxins are present?

(He can't get his hands on heptane or DCM or any cool solvents.
What is suggested here?)

:arrow: i figure 50g should yield a little less than:
1.5g bufotenine
0.4g 5-MeO-DMT
0.1g n,n-DMT

Thanks again,
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soulfood
#10 Posted : 2/24/2010 2:31:06 PM

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D_Juggz wrote:
Stop Stop

4) Run overnight with acetone 60-70ml
Quote:
69Ron: Acetone @ 20 C: soluble (5 g/100 ml)

5) Add vinigar to salt out bufotenine.
6) Pour off acetone, and let it dry out.


I'm a little confused about this bit. Unless you basify the seeds before the acetone wash this will just work as a defatting step and the alkaloids will remain in the seeds.

I'm also pretty sure even if you did rinse out the basified alkaloids with acetone, by adding vinegar you would be making bufotnenine acetate and all acetates I've come across are soluble in acetone.

Make sure you basify before you rinse the seeds and salt out the goods with citric or fumaric acid.
 
ThirdEyeVision
#11 Posted : 2/24/2010 3:27:43 PM

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I agree with soulfood about basifying prior to alk pull. A defat wouldn't be a bad idea though. Let us know how your friend does.

Your friend might want to throw some DE in the soxhlet with the powdered seeds.
ThirdEyeVision
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soulfood
#12 Posted : 2/24/2010 4:21:26 PM

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A previous defat wouldn't hurt, but the salting out is an adequate defatting step in itself which in my experience is more than adequate.
 
D_Juggz
#13 Posted : 2/25/2010 12:56:43 AM

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Thanks for the quick responses, we are all here to learn. Could someone please explain, how the pka of bufotenine works? eg, basified it is soluble in Acetone, but acidified (but not acetate) it is insoluble in acetone. How about IPA? same deal?

1) Toast seeds, snap in half first.
2) Grind seeds in a herb grinder untill fine
3) Put powder in soxhlet, using a cotton bud as a stopper top and bottom.
4) Run overnight with basified acetone 60-70ml (NaOH?) + (DE)
5) Add Citric acid to salt out bufotenine. --This would work right?
6) Pour off acetone, and let it dry out.
7) Convert the left over solids back to Bufotenine freebase by adding a spoonful(2g) of Sodium Carbonate and just enough water to turn them into a pasty consistency. Dry completely.
8 ) load into soxhlet and pull with IPA over night.
9) reduce solvent via distilation.
10) evap remaining IPA


What is DE, sorry?
The hardest thing of all is to find a black cat in a dark room, especially if there is no cat.
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soulfood
#14 Posted : 2/25/2010 1:11:12 AM

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I've added some changes here:

1) Toast seeds, snap in half first.
2) Grind seeds in a herb grinder untill fine
3) Add 1 part sodium carbonate to 4 parts seeds material then moisten enough to make a paste.
4) Allow to dry then grind to a powder
3) Put powder in soxhlet, using a cotton bud as a stopper top and bottom.
4) Run overnight with acetone 60-70ml
5) Add Citric acid saturated acetone to salt out bufotenine.
6) Pour off acetone, and let it dry out.
7) Convert the left over solids back to Bufotenine freebase by adding a spoonful(2g) of Sodium Carbonate and just enough water to turn them into a pasty consistency. Dry completely.
8 ) load into soxhlet and pull with IPA over night.
9) reduce solvent via distilation.
10) evap remaining IPA


 
D_Juggz
#15 Posted : 2/25/2010 1:46:55 AM

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awesome! and the sodium carbonate in 4. basifies it enough to be soluble in the acetone - good idea!
SWIM can't wait to try this method!

I WOULD Like 69Ron's opinion since he probably has tried this before...
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g13juggalo
#16 Posted : 5/21/2010 6:25:39 PM
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Any way one could do this, but only using acetone as a solvent, as well as whatever one would need to basify?
 
ThirdEyeVision
#17 Posted : 5/21/2010 6:29:57 PM

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g13juggalo wrote:
Any way one could do this, but only using acetone as a solvent, as well as whatever one would need to basify?


Yes. Bufotenine freebase is soluble in acetone. So do the above but replace the IPA for Acetone.
ThirdEyeVision
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g13juggalo
#18 Posted : 5/23/2010 3:16:15 AM
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Ahh. Thanks.

Any way one could basify it in one step? It seems unnecessary to do it between so many steps. and would the last pull be necessary, or is it just to clean?

and where should I get citric acid?
 
 
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