can simple A/B convert n-oxide to freebase?

[picatris]

SWIM had a dish with a slim film of n-oxide (or what he believed was n-oxide) from a MHRB extraction done sometime ago. The dish was in open air for 2-3 months in the air, always yellowish and greasy, but SWIM always thought that one day he might get something out of it, as the thing had that unmistakable smell.

So last week he decided to clean the material for some new extraction, yet he decided to see what he could get out of the dirty dish. Having zinc or other reducing agent at hand, he decided to use the scrapings in a hot A/B "extraction". Being lazy and somewhat distrustful of the process he forgot to weight the oily stuff, but it was a smallish amount, no more than .2 grams, but as he never weighted n-oxide he can't be sure. Thus he warmed the goo in a 150 ml HCl solution at pH 3, and heat it up without boiling. Everything dissolved in the acid. Then he lowered the pH to above 14 with lye and did a 3 pulls warm naphtha extraction, measuring 40 ml of naphtha in total. After 3 days in the freezer, behold!, white crystals! The naphtha solution in the end was somewhat "milky", but was not tainted yellow. The crystals when dried weighted 50 mg.

Now what do you think? could simple A/B be a procedure for converting n-oxide to n,n? What is the chemical basis for such an assumption?

 

[amor_fati]

SWIM thinks it's possible that a small amount of DMT n-oxide can prevent pure DMT from crystallizing properly. What he would imagine happening is that the process simply isolated the DMT n-oxide from pure DMT that was trapped in the oil. How was the original n-oxide retrieved before being left out for so long?

 

[picatris]

SWIM thinks it's possible that a small amount of DMT n-oxide can prevent pure DMT from crystallizing properly. What he would imagine happening is that the process simply isolated the DMT n-oxide from pure DMT that was trapped in the oil

That's a possibility. Never occurred to SWIM that some spice might actually never crystallize and get dissolved in the other non-polar stuff caught by naphtha

How was the original n-oxide retrieved before being left out for so long?

The n-oxide (or rather the oily residue) was retrieved by evaporating the remaining naphtha after a crystallization, in order to get the most out of spice. As only oil was produced, SWIM left his evaporating dish lying around. He never cleaned, because of the strong smell of spice it produced.

Interestingly on this last operation (getting the n,n out of the oil), the naphtha became very clear with no yellow taint whatsoever, meaning perhaps that at least the operation isolated the oils in the polar solution...

 

[amor_fati]

Another possibility is that SWIY's naphtha may not be the cleanest to evap?

For future reference, if SWIY worked that oil around a bit, it would probably begin to solidify.

 

[picatris]

Another possibility is that SWIY's naphtha may not be the cleanest to evap?

For future reference, if SWIY worked that oil around a bit, it would probably begin to solidify.

I just can't understand what you are trying to say, sorry! :? In any case SWIM has triple checked (really) that his naphtha evaporates cleanly. Not even smell remains.

 

[endlessness]

he means if you keep scrapping and moving around the oil, it can very possibly start hardening up.. Sometimes there's residual solvent trapped under the outside layer of the oil, which keeps it from solidifying, and then when you scrape it and move it around it helps exposing this remaining solvent to the air and then it hardens up.

 

[amor_fati]

he means if you keep scrapping and moving around the oil, it can very possibly start hardening up.. Sometimes there's residual solvent trapped under the outside layer of the oil, which keeps it from solidifying, and then when you scrape it and move it around it helps exposing this remaining solvent to the air and then it hardens up.

Exactly. This can be observed clearly right before your eyes within 10-30min as a color change and a thickening, and the next 20-30min can be spent working it into a hard chunk of clay-like material.

 

[picatris]

Exactly. This can be observed clearly right before your eyes within 10-30min as a color change and a thickening, and the next 20-30min can be spent working it into a hard chunk of clay-like material.

In the first place let me thank you endlessness and amor_fati for all your help. This is indeed a great forum to learn!

Yet (yes, SWIM is thick!), SWIM is still trying to understand why the hardening of the oil might be important. This oil never hardened no matter how much SWIM scraped and moved it. It was always sticky even in somewhat low temperatures (17 C). SWIM's managed to use a kitchen rubber scraper to get it out from the dish, yet it was difficult to get the stuff from the scraper as it was like glued to it like tar.

So to get it straight:


1.1 A oily residue that might become thick with constant scraping means that (please fill in)

1.2. A oily residue that is sill like tar even after a long time and lots of scraping means that (please fill in)

2. Getting spice, or something really, really, like n,n out of that gunk means that (remove what's not relevant):
A. n,n, was trapped there in the oil, and A/B extraction got it together
B. there was some n-oxide that was converted into n,n with A/B performed
C. hmmmm, such a bad experience, it's hard to tell
D. It's not n,n SWIM's got. It's ________ (please fill in)
E. Other (please specify)

Sorry for being so Cartesian. This is not one my finest moments

 

[amor_fati]

1.1 A oily residue that might become thick with constant scraping means that (please fill in)

There's crystallizable substances contained, substances other than DMT n-oxide.

1.2. A oily residue that is sill like tar even after a long time and lots of scraping means that (please fill in)

This details a bit about how it's done: Amor fati's Approach to Freebase Spice Conversion - DMT-Nexus Wiki You've really got to put some elbow grease into it and give it at least an hour of work. That second one, especially, started out as a clear, thin, yellow oil and dried up quite nice as pictured. The first procedure helps give a picture of what it looks like during stages of the process. The conversion and washing steps wouldn't pertain in SWIY's case, of course.

2. Getting spice, or something really, really, like n,n out of that gunk means that (remove what's not relevant):
A. n,n, was trapped there in the oil, and A/B extraction got it together