xylene -> vinegar = water soup, help?

[m1nt]

Hi
Sorry for the quick summarization, in a hurry.

So SWIM started with 450g MHRB, did 4-5 naptha pulls.

After successful naptha pulls SWIM started to pull with xylene.
Because of the obvious smells of xylene SWIM tried to find another
way. Took 2 combined pulls of piss colored xylene and mixed with
%5 distilled vinegar x3 and water x1. SWIM then put combined vinegar
and water in a glass pot and continued to boil solution down to an orange
goo. SWIM than added (dropwise) a solution of sodium carbonate + water
and placed in the fridge for 48hrs.

Accidently froze the water in the mix, SWIM doesn't even know how I ended up
doing it this way, just something found reading peoples posts and decided
to try it. What can SWIM do to get the jungle/nndmt back to freebase form and
crystallized? SWIM wanted to avoid having to evap the xylene.

SWIM has 2 more pulls of xylene and would like a step by step procedure on
what should be done to recover the jungle spice and make it into crystals.
It seems that this information is very spread out and SWIM messed up somewhere
along the lines.

Thanks in advance,
c

 

[m1nt]

SWIM scraped up all of the hardened goo on the sides of the glass dish
and smeared it on a plate.

SWIM is almost positive there is still some regular n,n-DMT as
well as jungle mix.

This goo is still (obviously) mixed with sodium carb.

What should SWIM do with the scraped up goo to obtain freebase
xtals? Should SWIM do some naptha pulls so that SWIM may ultimately
get the red/orange crystals?

Also in pic #2 is a plate with the first xylene pull left to evap.
No more smell of xylene, is there anyway to collect this and re-x
a faster way?

Thanks,
c

 

[benzyme]

I don't see anywhere in your post where you mention basifying.
there's no reason to refrigerate or freeze anything but the nonpolar, after you've separated it from the basic phase.

the typical work flow is acidify --> defat with a nonpolar (optional..you save the acidic phase, that's where the alks will be, not in the nonpolar) ---> add base to the acidic phase---> add nonpolar, mix well---> separate the nonpolar---> freeze precipitate or evaporate.

do you have a stronger base? sodium carb is pretty weak.
I'd dissolve that goo in warm acid, and rebasify with a strong base, because chances are,
you will still have salts in that goo which will not migrate to the nonpolar phase.

 

[m1nt]

SWIM has xylene, naptha, heptane & diethyl ether mixture, %5 distilled white vinegar,
epsom salts, baking soda, sodium carbonate, lye.

That is what SWIM has to work with currently.

And sorry SWIM did not clarify on the specifics of the earlier
parts of the extraction. Was basified with 1g lye per 1g MHRB.

Also after 3 naptha pulls 75g lye was added to estimated amount of
water, and then added to the mix after it was allowed to cool.
This was then left 24hrs to allow it to work on the MHRB.

After 24+ hrs had passed, 1 more naptha pulled was executed.
After naptha pulls, continued on with xylene.

Thanks,
c

 

[benzyme]

why would you add xylene after adding naphtha? just curious..

you could use just xylene, it pulls better, but then you'd need to salt it out because DMT is so soluble in it that freeze precipitation isn't really an option, and xylene has a high boiling point. I'd use one or the other, adding xylene to naphtha will make precipitation more difficult.

 

[m1nt]

Your not being much help.

I pulled 3-4x with naptha.

Let batch sit out so remaining naptha was evapped off of the
top.

Then I proceeded to use xylene to do 4 more pulls
so that I could obtain jungle spice (and other misc alkaloids)

I will ask again because apparently the first 3 times it was not
understood, you said "I'd use one or the other, adding xylene to naphtha will make precipitation more difficult." I have asked multiple times, how can I precip.
the xylene without having to do a regular evap?

 

[benzyme]

and I told you, it will be difficult to get it to precipitate, you might as well salt it out.
you're doing things the hard way.

 

[jamie]

why did you add sodium carbonate?

All you had to do was evaporate the vinegar water solution until you cannot smell the acetic acid any longer..then you have freebase. The acetic acid vapes away.

 

[benzyme]

it would actually leave acetate salts.
I'm just confused why anyone would use sodium carb for anything other than
washing the polar compounds out of the nonpolar solvent. too many solvents being used here, leading to even more confusion and impurities. in any event, what that looks like is a supersaturated solution, which would need to be redissolved in hot aqueous phase, either acidic or basic, and reprocessed.