Any synthesis for nitazenes?

MadHatter

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Interesting and emerging benzimidazole mu-receptor antagonists. I'd love to see a write-up on the synthesis of any of the nitazene compunds from as available precursors as possible. Seen these pop up on darknet markets from time to time, usually from sellers that are obvious chemists selling off a temporary batch before disappearing into the woodwork, like true pros.
 

MadHatter

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Especially interested in clonitazene. Unlike other potent nitazenes like metonitazene that are known to absolutely skyrocket one's tolerance this one has not proven to develop any tolerance in a 35-day trial (G.Bromig, Klinishe Wachenskrift, 960-963, 1958).
 

MadHatter

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Actually, I found this write-up on Reddit. Anyone have any feedback on it?

https://www.reddit.com/r/TheeHive/comments/eyu1g3
Synthesis metonitazene, Etazene, etonitazene, clonitazene and other nitazene derivatives


The synthesis of nitazene derivatives is described in the US patent 2935514. The described method can be done nitazene, etonitazene, clonitazene, metonitazene, ISO, etazene and several others. During my scientific work, I have made 12 nitazene derivatives.
Etazene had the best recreational properties and this is my # 1.
I explained the synthesis route earlier:post: https://www.reddit.com/r/fentanyl/comments/ela9fa/_/Image : https://ibb.co/h2SZcbP (road from nitrile)


1 Synthesis benzimidazole (or nitrobenzimidazole) intermediate
Dry gaseous HCl acid is introduced into a molten mixture of (0.11 mol) of substitutes benzyl cyanide (Note 1)[in this case I use p-methoxybenzyl cyanide] and 11.6ml of absolute ethanol at 15-25*C until the latter is saturated.

After allowing the reaction mix to stand for 12 hours at 20*C the crude imino-ether hydrochloride (photo1) is taken up in 200ml of absolute dioxane and stirred with 15.2 g (0.1 mol) of 2-amino-4-nitroaniline (Note 2) for 2 hours at RT (photo2).
Then under reflux for 14 hours (photo3). From the still-hot solution the hydrochloride of 2-(p-methoxybenzyl)-5-nitrobenzimidazole precipitated by adding ethyl acetate saturated with HCl acid and then filtered immediately.
The freebase is liberated from the hydrochloride by boiling with aqueous ammonia solution, filtered and recrystallized from ethyl acetate. The resulting 2-(p-methoxybenzyl)-5-nitrobenzimidazole (photo4) was used in the next stage.

2**.Synthesis nitazene derivatives (N-alkylation benzimidazole)**
9g (0.066 mol) of diethylaminoethyl chloride in 10 ml of dioxane are added dropwise at 70*C to a stirred solution of (0.033 mol) of 2-(p-methoxybenzyl)-5-nitrobenzimidazole and 1g Benzyltriethylammonium chloride in 65ml of 1N NaOH (Note 3)(photo5) . The mixture is stirred for 1 hour at RT, the precipitated oil in taken up in ethyl acetate. The EtAc solution is extracted with dilute HCl acid, the acidic solution is rendered alkaline with NaOH and extracted again with EtAc. The EtAc solution is washed with water and dried with anhydrous potassium carbonate and evaporated. It gives 9g of a mix of 1-(beta-diethylaminoethyl)-2-(p-methoxybenzyl)-5-nitrobenzimidazole and 1-(beta-diethylaminoethyl)-2-(p-methoxybenzyl)-6- nitrobenzimidazole (Note 4).
This mix is separated into its two components as such:The mix is taken up in alcohol and is mixed with the calculated quantity of HCl acid in ethyl acetate and inoculated with the HCl of the 5-nitro derivative. After filtering and recrystallizing the resulting precipitate from ethanol, there is obtained 4.2g of pure 1-(beta-diethylaminoethyl)-2-(p-methoxybenzyl)-5-nitrobenzimidazole hydrochloride.
The mother liquor is evaporated, taken up in water, rendered alkaline with NaOH solution, extracted with ethyl acetate, and the extract is washed with water and dried with anhydrous potassium carbonate. The solvent was evaporated and then the crystals were recrystallized from a mix of ether and pet. Ether with inoculation of the 6-nitro derivative, pure 1-(beta-diethylaminoethyl)-2-(p-methoxybenzyl)-6-nitrobenzimidazole.
-------------------------------------------------------------

Note 1.
Substitutes benzyl cyanide, If you use:
4-chlorobenzyl cyanide you will receive an benzimidazole intermediate for clonitazene
4-ethoxybenzyl cyanide you will receive an benzimidazole intermediate for etonitazene
4-methoxybenzyl cyanide you will receive an benzimidazole intermediate for metonitazene
4-isoproxybenzyl cyanide you will receive an benzimidazole intermediate for iso.

Note 2.
2-amino-4-nitroaniline you can replace 1,2-phenyldiamine and use 4-ethoxybenzyl cyanide - you will receive an benzimidazole intermediate for etazene.

Note 3.
In the original patent, they did not use a catalyst. The catalyst facilitates the dissolution of the substances. It has a positive effect on the reaction speed and yield.

Note 4.
If you are doing etazene then you have no problem with isomers. You already have a product that can be used 😉
 

G.Patton

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Why don't you add photos from Reddit? Also, Insert the picture of synthesized substance formula. It's easy to understand with pictures.
 

MadHatter

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I'm sorry, but I don't see any alternative for editing the post?
 

MadHatter

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I'll add the photos here. Just to be clear: I haven't tried this synth and the pictures are not taken by me.

PHOTO 1:
UzM5oGEd6B

PHOTO2:
TRipCQOSmL


PHOTO 3:
KLJi1a2GPX


PHOTO 4:
1R4J3FSLkW


PHOTO 5:
KlHM7Eef0g

And the ingredients list:

Specialized chemicals:
1 of benzyl cyanide variants:
4-chlorobenzyl cyanide (for clonitazene)
4-ethoxybenzyl cyanide (for etonitazene)
4- methoxybenzyl cyanide (for metonitazene)
4- isoproxybenzyl cyanide (for isonitazene)
2-amino-4-nitroaniline

diethylaminoethyl chloride
Benzyltriethylammonium chloride

Stock chemicals:
Absolute ethanol
Absolute dioxane
HCl gas (NaCl and concentrated sulphuric acid)
Concentrated HCl solution
Ethyl acetate
Aqueous ammonia
Sodium Hydroxide
Anhydrous potassium carbonate
Diethyl Ether
 
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woohoo

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Great!
Much easier than fent, i want to try this.
Although, it's required more safety on last stage.
With fent you just add anhydride to anpp (also toxic, but much weaker than any fent derivate) and then you can easily transfer yield directly to diluting agent, without contamination.
And burn or dip plastic ware in oxidizing agents (small disposal glove box is a good thing).
Use thick cloth thread to get clear solution without hot spots and oily drops.

With nitazene's last stage accidents is possible, more serious safety is needed.
Disposal glove box isn't enough for strong derivates.
 

MadHatter

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Great!
Much easier than fent, i want to try this.
Although, it's required more safety on last stage.
With fent you just add anhydride to anpp (also toxic, but much weaker than any fent derivate) and then you can easily transfer yield directly to diluting agent, without contamination.
And burn or dip plastic ware in oxidizing agents (small disposal glove box is a good thing).
Use thick cloth thread to get clear solution without hot spots and oily drops.

With nitazene's last stage accidents is possible, more serious safety is needed.
Disposal glove box isn't enough for strong derivates.
woohooI'm sorry, could you elaborate? What is the perceived danger? Involontary ingestion or transdermal intoxication or what? Explosion?
 

woohoo

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Probably, a new bestseller with high potency and long lasting effects.
Dangerous shit! 200x potency of morphine and ~3 hrs of action.
(WARNING: OPIOID USE GLORIFY SHIT, I WARNED YOU)

Etomethazene, appeared on drug market in the 2022 spring.

(methyl instead of nitro group, maybe can be tuned to even more acceptable way)
https://www.reddit.com/r/Opioid_RCs/comments/tp8ajr
And, also i found this on wiki, very simple way to zenes (no need for nitriles or phenylacetic derivates)
800px-Etonitazene_2011_synth.png


Sounds damn dangerous, like new epidemic.
I posted it only for "education".
 
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MadHatter

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Yes, it's been "emerging" for a couple of years now. I've seen user reports mainly on metonitazene, and it typically produces a massive tolerance quite quickly. That's very difficult to reverse. That's why clonitazene looks like a more interesting candidate, partly because the above study where no tolerance had been detected, but also because it's less aggressive with a weaker effect. Easier to handle.
 

WillD

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1. To a stirred solution of 2-(beta-diethylaminoethylamino)-5-nitroaniline (12.6g, 0.05 mol) and p-ethoxyphenylacetic acid (9.91g, 0.055 mol) in THF (50ml) heated a t 50*C was added EEDQ (12.4g, 0.05 mol)
2. After 24 hr, more EEDQ (6.18g, 0.025mol) was added with a final addition of EEDQ (12.4 g, 0.05 mol) after 72hr
3. The mixture was allowed to react at 50*C for another 120hr
4. Solvent was removed in vacuo, and approximately 6.6ml of 12 N HCl was added with stirring
5. The solution was extracted with CHCl3 (2x200ml) and dried (Na2SO4)
6. Solvent was evaporated in vacuo to give 21.6 g (100%) of etonitazene hydrochloride: mp 161-164*C
 
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BlackoutBird

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Does anyone have a synthesis for Butonitazene? Is it just subsituting a different chemical for the benzyl cyanide like the other variants?
 

plancklong

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If I wanted to synthesize etomethazene using the improved etonitazene synthesis that William Dampier so graciously provided, would it be something like this?:
IIxJPsoFtv
 

JustFuckMyShitUpFam

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Anyone got a vendor in the EU for zenes? Ive blown around 3 grand looking for them only to end up getting scammed. The opi state is sad and the RC scene even more so. But zenes are really only the future since there do not seem to be fentalogues... or if they are please let me know.

If you happen to wanna help please get at me at [email protected], I can also help you with some substances I won't mention here but they are strong potent opioids. But that can be discussed in private. I just want a legitimate zene vendor. :(

Tried Eto btw from the clearnet link. Strong stuff, hurts like fucking shit and makes me cry while snorting it. Not sure if its my tolerance but not that euphoric. Legit just puts me to sleep for a few hours lol. Pretty like taking a strong benzo lmao.
 

epson

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Anyone got a vendor in the EU for zenes? Ive blown around 3 grand looking for them only to end up getting scammed. The opi state is sad and the RC scene even more so. But zenes are really only the future since there do not seem to be fentalogues... or if they are please let me know.

If you happen to wanna help please get at me at [email protected], I can also help you with some substances I won't mention here but they are strong potent opioids. But that can be discussed in private. I just want a legitimate zene vendor. :(

Tried Eto btw from the clearnet link. Strong stuff, hurts like fucking shit and makes me cry while snorting it. Not sure if its my tolerance but not that euphoric. Legit just puts me to sleep for a few hours lol. Pretty like taking a strong benzo lmao.
JustFuckMyShitUpFamrechemco.to has metonitazene in 1:3 or pure. Prices are very good and the quality is also good
 

tonymontana2023

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rechemco.to has metonitazene in 1:3 or pure. Prices are very good and the quality is also good
epsonHi am also looking to buy this product, could you please let me know, for a heroin addict who uses ~20% afghan freebase, how much more would you cut the product?

Thanks for your time!
 
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