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25I-nbome cleaning and wash?

K

klondike_bar

Bluelighter
Joined
Apr 18, 2012
Messages
135
I have received a quantity of 25I-nbome that was identified by the lab as being a botched synthesis (thankfully before i conducted my tests). It purportedly contains 40% 25I-nbome (unsure if HCl form yet) and a lot of intermediates.

I dont yet know what the raw materials are, and am hoping the lab can identify them. But i want to try and seperate the 25I from the materials to the best extent possible.

what is 25I-nbome HCl NOT soluble in? anything with water or ethanol cant be used, as it will absorb the nbome and likely the intermediate materials. I was wondering about naptha though, anyone have knowledge or insight?
 
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okay, so little update/insight.

i took 1g out, and dissolved into 10mL of ~80% alcohol. Took small amount of heat to accomplish, then stayed in solution even when cooled slightly. I now suspect 25I-nbome is soluble at well over 100mg/mL. 99% of the substance dissolved, and some small white flake-like particles remained that did not seem readily soluble.

evapped it out in a dish quite easily, but i still have far more than i desired. (goal is to remove >30% of the mass, which is intermediate forms of the 25I-synthesis)

From Cimbi synthesis reports, I imagine the intermediates could include:
1,4-diiodo-2,5-dimethoxybenzene (effectively insoluble in water)
2-(2-isopropoxy-5-methoxyphenyl) ethanamine
CMeOTf
TFA (solubility in water: miscible)(good solubility in organic solvents)
NaBH4 (The compound is insoluble in ether, and soluble in glyme solvents, methanol and water)
Boc2O (insoluble in water, soluble in most organic solvents)


i think that i need to do this as at least 2 steps:
1)dissolve into water, seperate and evap. dump anything that didnt dissolve
2) dissolve in solvent such as ether (or naptha, bestine, or toluol?) and *if less than 1/2 of mass dissolves - ie: nbome doesnt* dump the saturated solvent.

id love to hear opinions from anyone with a background in organic chem and/or synthesis.
 
You could try a liquid-liquid extraction to get rid of most non-basic compounds and then a recrystallization. To maximize your yield take into consideration the large apolar surfaces of the molecule when choosing amounts of solvents.
Do you have access to thin layer chromatography? This would be very useful to monitor the cleaning process.

I hope you have all the expertise and safety equip that's needed for that task. Don't splatter around too much, if you know what I mean 8(
 
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Bin it and blast the lab on SoS. No respectable lab should be putting this out. they will send you a replacement.

I would probably run an A/B extraction and be happy with that. Those chemicals are unlikely to do much harm with amounts less than 1mg.
 
Transform said:
Bin it and blast the lab on SoS. No respectable lab should be putting this out. they will send you a replacement.

I would probably run an A/B extraction and be happy with that. Those chemicals are unlikely to do much harm with amounts less than 1mg.
Click to expand...

the lab is who instructed me that the package they shipped was a bad snth before it even arrived. they shipped a replacement immediately and i am 100% satisfied by thier response.
 
That's really creepy.
RC's scare the hell out of me now after pounding a few grams of them down. 8(
I probably have no idea half the stuff I've taken.

Orders have included different consistency powders in the same bag before. Makes you wonder.
 
^I think you can be pretty certain that most RCs out there - especially the ones from the most reputable vendors - are as advertised. Vendors and labs are fully aware that there are people in the scene who will take it upon themselves to conduct analytical testing to determine the exact identity of each batch of compound, and report on any findings on infamous forums dedicated to feedback and scam reports. There is, through this tacit agreement, a kind of quality control which goes on in the RC scene.

The vendors you need to watch out for the most are the notoriously sketchy ones selling compounds under brand names ("benzo fury", "plant food" etc.). There have been numerous instances where such vendors have been caught red-handed selling either cut or blatantly misrepresented mash-ups of compounds which do not fit the description as sold.

Everything I have ever bought and consumed over my years purchasing in the RC scene has been high quality, with each new compound fitting the anticipated effects profile. It's quite obvious in testing them that they are indeed the compounds advertised.
 
From Cimbi synthesis reports, I imagine the intermediates could include:
1,4-diiodo-2,5-dimethoxybenzene (effectively insoluble in water)
2-(2-isopropoxy-5-methoxyphenyl) ethanamine
CMeOTf
TFA (solubility in water: miscible)(good solubility in organic solvents)
NaBH4 (The compound is insoluble in ether, and soluble in glyme solvents, methanol and water)
Boc2O (insoluble in water, soluble in most organic solvents)
Click to expand...

This stuff is from the radiotracer precursor prep.

You're more likely to have 2C-I and the N,N-bis(2-methoxybenzyl)-compound
 
Cortexiphan said:
This stuff is from the radiotracer precursor prep.

You're more likely to have 2C-I and the N,N-bis(2-methoxybenzyl)-compound
Click to expand...

thanks for the insight. cant find much info on that N,N,-bis compound though.

i tried a non-polar solvent (bestine) yesterday, and the bulk if not all of the powder failed to dissolve in it. I havent weighed the remaining powder, but i feel like between water+ethanol and bestine there is still more mass then desired.

If some of that mass is 2C-I as suggested, the issue isnt as big, though id like to know about that other compound.

the lab identified the issue and remediated it immediately for it. while its unfortunate the discovery occured after they shipped, their response to it was phenomenal. Theoretically i can dump this half-mixture and it wont be any loss to me, though if i could clean it, it would mean a good deal of extra compound :)

any other ideas for seperating? its a homogeneous mixture, so sifting/filtering wont work, and ive tried several solvents. i can only think of trying with just water (not alcohol), though i dont expect it to be different, other than a long evap time and needing 15ml+/gram.

my main concern is the safety of what else is mixed in. i can accept if it is reduced potency/activity, and simply max mixtures with more of this batch, but i will not do that if theres any reason that the uncompleted chemicals inside could be harmful or toxic.
 
Bestine, won't dissolve anything but perhaps excess benzaldehyde.

If you have a mixture of the three aformentioned amine hydrochlorides then A/B extraction won't work but it would remove inorganic and non-basic organic impurities.

The obvious choice is chromatography but I sense that is not an option. Recrystallization is probably the best choice. I would try dissolving in something like hot IPA and then adding xylene or bestine until something starts crashing out and then leave to cool down. This might get rid of the N,N-bis compound.
 
You have a powder with 40% 25-i and 60% unknown chemicals, you can wash it or filter it as many times as you want but in the end you won't know fuck all about what you have achieved without a costly lab analysis.

But on the other hand...25i is active in ug, so 40% isn't that bad, just increase the dose by 60% if you are willing to risk or know the other chemicals included are not dangerous....it's not like you will be consuming 500mg of some unknown chemical, more like 1mg.
 
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