• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Question about Bestine instead of Naphtha.

Migrated topic.
logos2012

logos2012

Rising Star
SWIM was wondering if one used Bestine/Heptane instead of Naphtha for a pull out of basified water, does one heat up the Bestine just as Naphtha? SWIM knows that Bestine's evap temp is lower than Naphtha so it would probably heat a lot quicker but SWIM was just wondering if heating up the Bestine would work better for a pull than not heating it up.
 
Sort by date Sort by votes
69ron said:
If you do all the extraction steps with DCM and then freeze precipitate using heptane, you’ll get the best yields with the least amount of time.

But if using DCM to extract from Mimosa, you must freeze precipitate using either heptane or naphtha to get clean white DMT crystals. If you don’t you’ll end up with a sticky slightly yellowish goo containing a mix of alkaloids. Generally, mixed alkaloids will often not crystallize until they are separated. DCM extracts more than just DMT. It extracts the so called “jungle spice” as well as all the DMT N-Oxide, both of which are insoluble in naphtha and heptane, and both are very active.
Click to expand...

Swim likes this idea and imagines performing an A/B with DCM followed by a quick sodium carbonate wash followed by reX/freeze precipitation with hot heptane (with NO defat performed).

Tell me if he has this correct.. The precipitate which would be filtered off would be clean nnDMT... Left in the Heptane would be jungle spice, small amounts nnDMT as well as DMT N-Oxide as well as a bunch of oil and gunk.

After evapping the leftover heptane, he could then reacidify, defat, basify, extract once again with DCM and do a quick wash to allow him to evap a combination of cleaned up jungle spice/DMT N-oxide combo.


He could then dry out the leftover plant material, and perform a STB on it, pulling with Toluene ... (OR SHOULD HE CONTINUE USING DCM HERE AS WELL???) and going on to clean as stated above with a quick wash as well as hot heptane recrystalisation etc....


Will the DCM be just as good as pulling the jungle spice as toluene?
 
Upvote 0 Downvote
monkeyboy said:
69ron said:
If you do all the extraction steps with DCM and then freeze precipitate using heptane, you’ll get the best yields with the least amount of time.

But if using DCM to extract from Mimosa, you must freeze precipitate using either heptane or naphtha to get clean white DMT crystals. If you don’t you’ll end up with a sticky slightly yellowish goo containing a mix of alkaloids. Generally, mixed alkaloids will often not crystallize until they are separated. DCM extracts more than just DMT. It extracts the so called “jungle spice” as well as all the DMT N-Oxide, both of which are insoluble in naphtha and heptane, and both are very active.
Click to expand...

Swim likes this idea and imagines performing an A/B with DCM followed by a quick sodium carbonate wash followed by reX/freeze precipitation with hot heptane (with NO defat performed).

Tell me if he has this correct.. The precipitate which would be filtered off would be clean nnDMT... Left in the Heptane would be jungle spice, small amounts nnDMT as well as DMT N-Oxide as well as a bunch of oil and gunk.

After evapping the leftover heptane, he could then reacidify, defat, basify, extract once again with DCM and do a quick wash to allow him to evap a combination of cleaned up jungle spice/DMT N-oxide combo.
Click to expand...

No, not quite. There won’t be any “jungle spice” or DMT n-oxide left in the heptane. It would be left in the yellowish DCM extracted gunk. They are insoluble in heptane. After you extract with DCM, you get yellowish gunk. You then dissolve that in hot heptane (no hotter than 50 C). Only the DMT and oils dissolve in the heptane. The “jungle spice” and DMT n-oxide stay in the yellow gunk that won’t dissolve in the heptane. You then pour out the heptane, leaving the yellow gunk with the “jungle spice” and DMT n-oxide in it. You freeze precipitate the haptane to get the DMT only.

monkeyboy said:
He could then dry out the leftover plant material, and perform a STB on it, pulling with Toluene ... (OR SHOULD HE CONTINUE USING DCM HERE AS WELL???) and going on to clean as stated above with a quick wash as well as hot heptane recrystalisation etc....


Will the DCM be just as good as pulling the jungle spice as toluene?
Click to expand...

No, that won’t work. All the “jungle spice” will be pulled out by the DCM. DCM extracts everything. DMT, DMT N-Oxide, and the “jungle spice” are all many times more soluble in DCM than in toluene or xylene.
 
Upvote 0 Downvote
Thank you for clarifying that.

so then it would be considered a waste of time to perform a STB AFTER a regular A/B extraction with DCM?

SWIM was under the impression that STB teks where good to pull even more after a traditional A/B was performed.

Lets say SWIM was simply looking to pull as much as possible, as cleanly as possible... the full spectrum of mimosa alkaloids- is an A/B done with DCM ALONE the best course of action?

Does he reacidify and perform a defat of the leftover DCM evap to get the other alkaloids? If so, what would be the best solvent to defat with? Is this the best way to clean up the DCM extracted goo?

OR.... does he simply extract everything with the DCM... performing a defat right then and there before the basifying step, and then go on to wrestling with crystalization of everything after he has basified etc...?

SWIM has got the old A/B route down pat- he stepped away for about 6 years or so (back when most everyone was using ROSINOL!) and is now interested in dreaming about a full spectrum of alkaloids... as well as the higher yeilds that these 'recent' developments have his curiosity peaked.
 
Upvote 0 Downvote
SWIM says thanks for all your help! SWIM was wondering, if he was to do a sodium carbonate wash on the DCM before evaporating/distilling would the DCM sink to the bottom instead just as when pulling spice?

He wonders also if it is better to do the wash right after the pull with the DCM or is it better to evap/distill first then mix back in with bestine, seperate the nn from the other alkaloids and do the wash with bestine then freeze precip?
 
Upvote 0 Downvote
On to a more practical consideration of a kitchen chemist.

Seeing that the DCM sinks, lets say 500g of MHRB- finely powdered, is being processed, if the basified sludge is not being filtered, when the DCM is added, will some of the particulate matter end up sinking into the DCM or will it stay afloat in the aqueous layer?

Also... seeing as how this wouldnt be practical to be done in a sep funnel... does anyone have a good idea regarding the vessel in which this should be done, and the means for which to remove the DCM from the bottom?

Maybe swim shouold make a separate topic for this one.

He was thinking of perhaps fashioning a makeshift hose/stopvalve that could be screwed onto the top of a HDPE 2 container. This way agitation could be done, the valve possible screwed on and then the whole thing inverted, allowed to settle then the bottom DCM layer drained. At this point, a hole would have to be made in the top of the container so as to not have to worry about the container burping.

DCM along with basic materials and such... its ok for that type of plastic, correct?


Swim doesnt have to want to bother with filtering off large amounts of basified plant material
 
Upvote 0 Downvote
any suggestions regarding the vessel in which it is extracted then?

seems glass will suffer etching from the lye and plastics will dissolve... swims fantasizing about a 500gram extraction

Maybe one of them super-thick glass 5 gallon carboys they sell at wine/beermaking shops?
This means nalagaline and PET are probably also out of the question?
 
Upvote 0 Downvote
the "etching" of the glass with lye from a single extraction is negligible, especially if using borosilicate glass (i.e. Corning, Pyrex, etc.)

in labs, borosilicate glass is standard with all wet chem procedures, regardless of reagents used (except when using HF..hydroflouric acid will dissolve glass).

use either borosilicate, or stainless steel.
if unavailable, you can try with nalgene carboys.
you can always test plastics, to see if any degradation is visible
but don't assume HDPE plastic containers will be inert.
if plastic dissolves in the solvent, it may leave your product very messy, and nearly impossible to clean up. you'd rather run the slight risk of having etched glass bits (easily separated) vs. dissolved plastic
 
Upvote 0 Downvote
So SWIM was wondering, at what step in the DCM extraction process would it be best to do a sodium carbonate wash?

Would he wash the DCM liquid?

Evap the DCM then wash the yellowish gunk?

Use warm bestine to crash out the NN then wash the liquid bestine?

Or use warm bestine to crash out the NN then wash the spice after evaporating/freeze precipitating?
 
Upvote 0 Downvote
sodium carb wash can be done when dcm is added to the basic solution. let it settle, then add aqueous sodium carbonate. 5% (5g baking soda per 100mL water) should work fine. swirl, don't shake..then separate. evap the dcm, dissolve with minimal warm bestine and allow to evap at room temp for large crystals, or put the bestine/dmt in a vial in the freezer, and crash out for small crystals. yield will be the same, either way
 
Upvote 0 Downvote
Cool thanks! SWIM was also wondering, if he was to do a pull with bestine, then a sodium carbonate wash, would it make sense to recrystallize with bestine to remove non polar solvent impurities since bestine was originally the solvent used?

He says it just might not make sense since it soaks in the bestine to recrystallize anyway.
 
Upvote 0 Downvote
And Also a question for 69ron, you said, "Only the DMT and oils dissolve in the heptane." SWIM tried a pull with bestine after he had done a pull with DCM, he did a sodium carbonate wash on the liquid bestine then evaporated the bestine. The spice that was left was very yellow and had quite a bit of oil residue left in the dish. SWIM said the spice also smelled a lot like the DCM spice before the jungle and oxide are seperated. What are the oils that you were saying dissolve in heptane?

Is it possible that the bestine might have picked up some of the remaining DCM with the oils and stuff?
 
Upvote 0 Downvote
Back
Top Bottom