Small batch chemist looking to do the Henry reaction….

[Rabidreject]

Hi guys,
I’m curious if anyone on here would sell me relatively small amounts of a few different aldehydes so that with the help of both nitromethane and nitroethane I can explore the worlds of psychedelic amphetamines and PEA’s, without having to buy each different aldehyde in 500g quantities.
Im specifically looking for 3,4,5-trimeothoxybenzaldehyde and 2,5-dimethoxybenzaldehyde.
I definitely feel like I need to experience mescaline after all these years….but I certainly don’t want a few hundred grams of it lol
The 2,5 is a little different in that there seems to be more things I know how to use it for.
To be honest I was just going to make P2NP just so I could perform the Henry rxn but forgot about the primary amine needed and I certainly can’t find n-butylamine or cyclohexamine and tbh I’m not interested in the end product anyway so figured I’d save the nitromethane I recovered from a surprisingly 50:50 DCM:nitroEthane product for this country….

Aaannyway
I thought maybe someone may take pity on me ha!

 

[Osmosis Vanderwaal]

Someone posted a route to dimethoxybenzaldahyde and other substituted phenylethylamines, sounded pretty hard

 

[Rabidreject]

Yeah, I have read into it to be fair - I decided I have enough on my plate trying to get cyclohexylamine atm. I don’t fancy my chances of making the aldehydes. Your right it sounded pretty hard and I’m sure there is a reason people arnt doing it!
I doubt I’ll end up using the bottle of benzaldehyde tbh…

 

[Rabidreject]

Yeah I’m not suggesting I turn my benzaldehyde into anything else, either someone please sell me some n-butylamine or let me know if methylamine would work as I could potentially make a small amount. (Obviously with other materials)
I was really hoping someone would say yeh I’ll sell you 250g of each! The 2,5-dimeth/aldehyde and 3,4,5-trimeth/aldehyde more so than anything else. I guess it doesn’t matter I’ll probably end up buying 500 of each anyway.
im just saving to my nitroethane and nitromethane for the correct tasks

 

[The-Hive]

Ammonium Acetate Catalysis last option

 

[Rabidreject]

Okay so I’m trying to create mescaline. Can you elaborate a little on what you mean by ammonia acetate catalysis? I have googled and read a whole piece about primary amines but stil don’t really understand if I can just switch one out for another, I doubt it lol
The only synth iv read is the one on here that uses cyclohexylamine…however, don’t really know the cheapest way to obtain small amounts.
I thought the nitro was the bitch to obtain! Ha how wrong I was.
I would also like to make the corresponding TMA as well tbf but I can’t say Iv looked into it yet.
It’s really annoying when you want to make a gram of something ha it’s just not possible unless you make all reactants from scratch yourself.

 

[Rabidreject]

I’m in an annoying position where I know enough to know the molecular pathway people take, but any details I cannot work out on my own. It’s not like I’m doing it to sell it…
I’m still working on reductive amination of tryptamine but need dry ice and have been busy and unable to take receipt of it and proceed.
I just know enough now to know that doing things in small quantities is HARD

 

[Rabidreject]

Also following a Rxn without a rotovap is fairly hard in and of itself….

 

[CCL4 huffer]

i totaly disagree its shit easy a rotovap is only a convinience if u dont have time in my opinion. ive been doin chemistry for a long time now and i just use a normal destilation setup with a vacuum pump if necesary.
also why would following a reaktion without a rotovap make any difference??????

 

[Rabidreject]

Oops posted my reply by mistake in the general section but yes you are correct tbf…
I am lazy and am not a chemist but have learned an awful lot in the past 6 months it’s crazy.
All I’m here to do is learn.
Ah just read the post below lol anyway I agree with you tbf

 

[The-Hive]

Think you only need a weak base Ammonium Acetate,cyclohexylamine and n-butly could be wrong but can always try

 

[Rabidreject]

Ya ammonium acetate is going to be the one I would think….
I’m going to go for the 3,4,5-triMEOba before the 2,5-di. Purely because reacting it with nitromethane and you are on your way to mescaline and yet I’m still then free to try using the nitromethane to make the 3,4,5-TMA as well.
I do want to make 2c-b at some point but bromination scares me in general - I do have 1cc I bought ages ago that is stored in the vial it came in but using the gas sounds even more scary!!
Is there not a way to brominate something without using elemental bromine?

 

[The-Hive]

And this one

Successful 2C-B Syntheses

 

[Swirly]

Yes Rabidreject, bromination is no longer a problem. Pick up some NBS (N-Bromosuccinimide). But you need to have made clean 2c-h Hcl or 2c-h Oxalate. But it is not that difficult.

Now there is a non-toxic and safe synth to 2c-b you can do at home. NaBH4 + Cu(II)Cl reduction and NBS bromination. And it works well in fact even for larger amounts.

I will eventually copy/paste my write-up of 2c-b some time.

 

[Rabidreject]

The significance of this post has just hit home. Massive amounts of thanks for a few simple words! Haha

 

[Rabidreject]

Yeah okay I do agree with that - okay so I need a vacuum source that’s capable of running more than the 30 mins they said my oilless one can run for. I need an oil rotary vein pump. But yeh I am fairly lazy I’m not going to lie and recovery of solvents is always something I like to do where possible, so it’d be useful but okay not for direct rxns obviously.
That said, I was watching a pootube guy who released a 2,5-dimethoxy-b-nitrostyrene (I appologise as I probably butchered that spelling or way of writing but you get what I mean) and he accidentally added nitroethane instead of nitromethane but I noticed he didn’t have to add a primary amine, is that because the aldehyde is more complex than say benzaldehyde -> P2NP?
Listen, I am not a chemist, I am on here trying to learn, with a few bits and pieces that I have needed so far.
My hotplate/stirrer is knackered so that’s next to get updated but honestly, I’m finding the more I learn, the less I know!
I WAS thinking of getting the 3,4,5-trimethaldehyde, reacting it with nitroethane to get the corresponding TMA? (Post b-nitrostyrene)
OR reacting it with nitromethane (and the synth iv read says another primary amine - cyclohexylamine) to eventually (granted after a few steps AND the need for a vacuum) to arrive at mescaline.
Im working out what I should buy first, 3,4,5-trimeth aldehyde (sorry about the shortening of aldehyde names consistently on here, it’s pretty annoying to keep writing them) or 2,5-dimeth.
What do you end up with if you simply react 3,4,5-trimethoxybenzaldehyde with nitromethane? I assume 3,4,5-trimethoxynitrostyrene and then the phenethylamine 3,4,5-trimethoxyphenethylamine after reduction with LiAlH4 or whatever you choose to use…
Then its also not hard to instead react it with nitroethane and get the amphetamine as I mentioned earlier.

Am I totally mistaking things here?

I will admit I had next to no knowledge about 6 months ago and am currently trying the reductive amination of tryptamine to n,n-DMT but need to buy dry ice and carve (sorry for the punn) out the time.
I actually came on here to ask a little about LiAlH4. If one can’t find small amounts of it, Is an amalgam when someone uses aluminium to make it themselves? I hear this term banded about sometimes and never really knew what it meant….
I do have reducing agents at hand, I’m just curious.
thanks

 

[Rabidreject]

In other words, colour me confused

 

[Rabidreject]

Oh also, with regards the pump, I was simply doing some vacuum filtration the other day and the next time I saw my neighbour he thought I was sawing through the plumbing as I had it sat on the fucking kitchen surface! Idiot!
I did buy an aspirator from China but it doesn’t seem to pull a vacuum as of yet…fuck knows what I’m doing wrong or was sold a bunk or just can’t get adequate flow.

 

[Rabidreject]

Right now, I’m willing to concede I don’t need a rotary evaporator to conclude the n,n-DMT synth but I DO realise I need sufficiently cold temps (and to add things slowly) using dry ice and not just an ice bath in order to do it this time of year in my country….
That’s nothing to do with this thread though really - it’s just the reason I got into organic chem, not realising tryptamines were the more complex of the two main classes of psychedelics stupidly.

 

[Rabidreject]

So yeah, I figured 3,4,5-trimethoxyphenethylamine was mescaline.
The question is can I just react the corresponding aldehyde with nitromethane and then reduce to obtain mescaline?
Why, in the synthesis I read in this section do they utilise the cyclohexylamine?

 

[Rabidreject]

And at the same time do the same RXN with nitroethane to obtain the corresponding TMA (although I can’t say iv looked it up and think it to be a worthy drug to synth - I shall look it up in my copy of pihkal - but as stated before - lazy!

 

[Rabidreject]

Actually lazy isn’t the word coz I’m putting in quite a few hours studying these things I just feel like the more I know, the less I know ha

 

[Rabidreject]

Okay, iv gathered my thoughts and my main question now is what is the difference between the substance you obtain from reacting this aldehyde with nitroethane as opposed to nitromethane - I know the end result, but what is the difference in the nitrostyrene? Does one make a b-nitrostyrene and one a styrene? I don’t know and am not claiming to.
Essentially, what is the difference between the precursor to the n-styrene iv seen be produced using nitroethane and what is made from instead rxn with nitroMethane…this is what is confusing me atm but again I need to pull out pihkal

 

[Rabidreject]

Okay, iv gathered my thoughts and my main question now is what is the difference between the substance you obtain from reacting this aldehyde with nitroethane as opposed to nitromethane - I know the end result, but what is the difference in the nitrostyrene? Does one make a b-nitrostyrene and one a styrene? I don’t know and am not claiming to.
Essentially, what is the difference between the precursor to the n-styrene iv seen be produced using nitroethane and what is made from instead rxn with nitroMethane…this is what is confusing me atm but again I need to pull out

Basically, a pretty notorious among the chemtubers released a video today and he reacted 2,5-dimethoxy with nitroethane by accident instead of nitromethane. He planned to obtain the precursor n-styrene to 2c-b, however as he added nitroEhane instead he produced the precursor for 2,5-dimethoxyamphetamine - he never did the reduction to the amphetamine. (a pretty darn undesirable drug by all accounts)

If he had used the correct nitromethane would he have obtained the b-nitrostyrene for 2c-b?