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Bufotenine Extraction

Migrated topic.
Jorkest said:
when you tried to crystallize in acetone..how did you do it? did you just let it evaporate down?
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SWIM dissolved 100 mg of freebase bufotenine in 2 ml of acetone (the minimum required to dissolve it) at room temperature. He then evaporated it down to 1 ml using a little heat (about 40 C). Then he left the rest to evaporate at room temperature. It only took a few hours to get crystals from it. Note that this never worked with impure bufotenine. He needed 90%+ purity for this to work.
 
Jorkest said:
after MEK:heptane wash


left overs of MEK:heptane wash


this was all after the xylene boil
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The difference between those results and SWIM's must be the fact that SWIM’s starting material was from an A/B extraction using DCM (that included defats with DCM). So his xylene boil produced nearly pure bufotenine crystals. They were maybe 95% pure after the xylene boil.
 
that makes a lot of sense..hes pretty happy with the end product that he has..im sure he can even purify it more with a slightly different combo of MEK:heptane..add just a hair more heptane to get rid of some of the impurities..it wont be hard now that its fairly pure
 
these are the steps SWIM has taken so far to get the fairly decent crystals

1. freebase ground seeds with sodium carbonate and a dash of water
2. dry with magnesium sulfate
3. pull with acetone
4. precipitate with FASA
5. wash bufo fumarate with acetone
6. freebased with calcium hydroxide and some water
7. did not dry or pull with acetone(this is water, calcium hydroxide, and bufo fumarate) which became freebase bufo and water and some other stuff(not sure what)
8. boiled xylene (with the bufo mix) for about 6 minutes
9. poured off xylene from the bufo mix
10. let it cool(snow, freezer, then shelf)
11. collected the freebase bufo and tested it..it was very harsh..visuals not extremely impressive(he did smoke some last night though)
12. washed with MEK:heptane in a 2:3 mix
13. boiled off MEK and the heptane evaporated fairly quickly leaving a gooey film
14. collected the film and spread it over some glass and spread it out with a razor over and over again so that it would dry
15. collected what was left(picture above)

things he would have done differently

at step 2 he thinks he would just let it dry naturally instead of adding another substance

at step 7 he would have dried the freebase and mix and then pulled with acetone so that he would not be boiling water, calcium fumarate(whatever), and freebase bufo...the acetone would then have been evapped then boil in xylene

at step 12 he may slightly change the ratio of MEK to heptane..it seems that there is some slight impurities that come out..maybe a 3:5 ratio might work a bit better

at step 13 the MEK and heptane evapped fairly fast and maybe thats why there was a touch of yellow

so those are the steps SWIM took..he thinks they can be reduced a few but being his first time trying this there has been a few errors..but ones that have been able to be corrected...luckily
 
That's way too many steps. There must be a simpler way.

I’m thinking about this possible tech.

Step 1 – Grind and Dry
Coarsely grind 100 grams of fresh seeds. Dry in an oven at 250 F until completely dry.

Step 2 – Defat with Xylene
Boil seeds in 500 ml xylene for 5 minutes. Filter and discard the xylene. Repeat until the xylene comes out clear.

Step 3 – Freebase with Calcium Hydroxide (lime)
Add 1 part calcium hydroxide to 2 parts seeds. Add enough water to form a clay like consistency. Mix for 5 minutes. Dry in an oven at 250 F.

Step 4 – Extract Bufotenine Crystals
Boil seeds in 500 ml of xylene for 5 minutes. Filter out the seeds. Put aside the xylene to cool. Collect freebase bufotenine crystals in a few hours by pouring off the xylene.

SWIM has not tried this yet. He doesn’t have any more seeds. He believes this will work very well. If you defat with xylene, you pull everything out that’s soluble in the xylene. Then you freebase and extract the alkaloids in xylene. Only the bufotenine should dissolve in the boiling xylene. When the xylene cools, bufotenine drops out. It should work quite well. SWIM already ordered more seeds. But it will be several days before he can give this a shot.

Tell me what you think.
 
that looks very doable..he will try it on another batch of seeds..he has enough..once he has this one finished

its been quite the mess around trying to clean up this stuff..its too bad xylene is so nasty

but that tek looks really nice...simple and easy..SWIM has just been trying like mad to clean this stuff up but its been tough..
 
SWIM has never done this extraction before, but he is wondering if 500mL Xylene is necessary, since it will be thrown out. Maybe 100 grams of seeds has more volume than what SWIM thinks.

How many times has SWIY found he needs to boil the Xylene before it stays clear?

could SWIM use a blender on low setting to coursely grind the seeds? He has a coffee grinder but it's broke and he needs to send in for replacement. Burr grinders have a tendency to jam.

Appreciate the hard work.
 
there are lots of oils so its best to use as much xylene as possible..but SWIM is about to test this out and will get back to the thread
 
I don’t think anyone knows the answer to that yet.

Freebase bufotenine seems to be totally insoluble in xylene unless it's boiling. I would imagine that since the natural salts are far more polar and are practically insoluble in hot boiling acetone that they are probably completely insoluble in boiling xylene. But that is just a theory. The only way to know is to test it.

Once in the past SWIM tried to extract the natural salt actives from the seeds in a Soxhlet for 18 hours using boiling acetone. No actives were extracted. If acetone can't do it, I very much doubt that xylene can. Xylene is far less polar than acetone.
 
defatting is complete(good enough..will purify with MEK:heptane if there is any junk)

freebasing with calcium hydroxide


edit:
now drying
 
ok.. SWIM tried crystalizing from toluene. he dissolved about 2.5g of dark goo in 200ml toluene. after he heated, poured it off and cooled it the toluene turned from clear yellow to cloudy whitish yellow. he has now let it sit in the beaker over night.. its still cloudy but nothing has fallen out. this is lab grade toluene. it doesnt seem to work. or can it sometimes take longer for the crystals to fall out? how long does it take with xylene?
 
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