Looking to do a Henry reduction on 3,4,5-trimethoxybza…

[Rabidreject]

Hi guys,
I’m looking to make some mescaline, I have everything under control in terms of acquisition of chems apart from, the cyclohexylamine.
I had issues with the n-butylamine before which is why I havnt used my nitroethane for amphetamine at all.
dang primary amines…

Could this be switched out at all? Or can it be squired easily?

 

[Rabidreject]

I can easily get cyclohexylamine hydrobromide, would this work?

 

[Osmosis Vanderwaal]

You could deprotonate cyclohexylamine hbr with a base easy peasy, or make it from analine, but are you sure that's what you need and not phenylamine?

 

[Rabidreject]

I mean, the synth I was looking at on here said cyclohexalymine - I do have a big bottle of cyclohexanone as well.
Was thinking of doing the rxn with ammonia but the synth I’m reading used Zn powder - could I use something else? I am assuming all we are doing here is reductive amination? I say all…

 

[Rabidreject]

This is the ammonia rxn that I was reading. Have a look. Also I’ll post the link to the mescaline one but it’s the first you come across when looking through the phenethylamine / amohet section of the forum…

 

[HerrHaber]

The Henry reaction can be catalysed by even stronger bases such as NaOH, this procedure can be found on orgsyn about the synthesis of betanitrostyrene. I successfully applied this to 2,5-dimethoxy-betanitrostyrene and as far as I can remember proton nmr said it's ok.

 

[Rabidreject]

Oh nice. okay
It’s a couple of RXN’s I’m working up to. I want to make sure I have everything before I spend the money on 500g+ of the 3,4,5-aldehyde that’s all.
To be honest, the hardest thing to find so far has been the nitroethane and nitromethane. Luckily both were distillable in varying amounts from products. Annoyingly the nitroethane being slightly easier and less effort to distil - you lose so much to the azeotrope you end up with a lot of methanol/9% nitromethane but then you do also end up with nitroethane coming over in the end also - or at least I did. It certainly smells different yet stronger than that of the methanol/nitromethane mix and it weighs what it should for the ml.
It’s just a PITA having to do like 5L worth of distillation. Mind you it is how I got my ethanol I suppose.
Yeah ammonium acetate seems I treating as do stronger bases like KOH or even NaOH fuck knows if it would work though.
It just seems like the logical least complicated ones to start with mescaline and 3,4,5-TMA

 

[Rabidreject]

He says, fully aware he is going to retry the DMT reductive amination from tryptamine using dry ice and also not fucking up and using the wrong fucking solvent to re-x the goo (oil) I was left with, with. Does that even make sense?

 

[loadingST]

Amonium Acetate is perfect for the job with some GAA as solvent crystalization of the nytrostyrene is so easy with ice, or ethylamine or methylamine acetate works even more good

 

[Rabidreject]

Ice? I get the rest, not that I can really OBTAIN them - well I probably could in large amounts I don’t need from China. But I have everything I need to at least TRY the reaction to make cyclohexylamine - if shulgin used it, AND it saves me some nitromethane, both of those are very good things!
Having said that, YES, I have ordered some ammonium acetate as well.
I just need to work my way through the other like 3.5L of nitromethane containing fuel! Ha

 

[yuiopjkl]

I think he means ammonium acetate with GAA .
or you can synthesis cyclohexylamine
cyclohexanone → cyclohexanone oxime → cyclohexylamine

 

[Rabidreject]

Yeh both of these are in the wider plan….

 

[Rabidreject]

Yes but I have the GAA already!

 

[Rabidreject]

Yeh my plan is to just try both methods tbf.

 

[Rabidreject]

Can I ask if the ammonium acetate / GAA would work for the production of a small quantity of p2Np from benzaldehyde and nitroethane?
I can’t find n-butylamine which seems to be most people’s starter. It’s not something I’m as interested in as the psychedelic phenethylamines but I do feel like it may just be easier to make my own amphetamine adhd meds seeing as the shitty NHS ‘isn’t taking on more patients’ rediculous but hey ho. In small amounts? Any ideas? I have the benzaldehyde, I now have what I thought was the hard part which is the nitroethane, then re-looked at the synth and realised I’d forgotten the catalyst. Bah….and not like a sheep…like that Christmas dude!

 

[yuiopjkl]

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/p2np-syntheses-ammonium-acetate-catalysis.8786/post-42351

 

[Rabidreject]

THAT my friend, is the article/ post I have been looking for for a while. I’m hoping I can at least offset my ADHD and lack of motivation/ energy, in order to fuel further more psychedelic projects, using small quantities of amphetamine.
It would certainly be more useful than the bottle of benzaldehyde or any of the other chems listed!

I am a little worried about x’stallisation, however that’s probably something to do with the slop I’m left with after attempting to add NaBH4 too quickly (I’m actually assuming this - either that or it’s almost impossible to re-x from heptane - I’m going to try one last thing of adding a little ether also), before just restarting the whole thing and this time actually add my reagents slowly!

 

[Rabidreject]

I mean we do have some success in that I managed to obtain some REALLY clean looking crystals that do smell of DMT - trouble is, there is like 500mg of it! Thats probably being quite generous also!

The reason I have a feeling - well, I know it went up to like 5-10c at times, but the reason I think I may have created some sort of beta-carboline side product is that the methanol RM that’s left over glows pretty heavily under UV light.
I dunno I should have been doing TLC on it to be fair, in both the terms of testing but also giving it more attention and time when adding the reducing agent! Ha

 

[HerrHaber]

I wouldn't compromise the synthesis with doubtful nitro alkanes, especially if EU based.

 

[Rabidreject]

Yeah people keep saying that but I sided all my nitromethane from the EU and distilled it from a 40%w/w nitromethane;DCM mix, worked great for making b-2,5-DMONS.

The issue for me is finding each relevant catalyst for each aldehyde I want to perform the Henry reaction on….

I was thinking about trying the reductive amination of cyclohexylamine from cyclohex using, I believe, ammonia, zinc and CaCl2…

We’ll see - my backup is o jut buy a bottle but my dudes away at the mo anyway…

 

[HerrHaber]

Catalysts I worked with either heard often about are n-buthylamine, cyclohexylamine, ethylene diamine and even monoethanolamine. Ethylamine also works despite it being a 70% solution in water.