Small batch chemist looking to do the Henry reaction….

[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]

@Rabidreject check this out https://chemistry.mdma.ch/hiveboard/rhodium/2cb.beaker.html

 

[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]

Oh legend

 

[Rabidreject]

Although let me explain. I get paid by the government for various disabilities every two weeks and 85% roughly gets spent on my private medical cannabis bill.
I am trying to reduce this…taking too much too often is a big thing in my life - I am a recovering heroin (opiate) addict and primarily a benzo addict.
I am luckily prescribed buprenorphine for the opiate dependence - iv just started Buvidal sub-cut injections. At the mo I’m on weekly and it’s a bit of a rollercoaster
HOWEVER, I am getting there, slowly but surely.
As I have said before - chemistry is a way better drug than any of the drugs it produces, even if that is why I got into it. Not to make money but to learn more about the non addictive - maybe even anti-addictive drugs and the first that came to mind (knowing nothing about chemistry was DMT) so I got some hardware and a load of chems and this and that and iv ended up with quite a bit but more than that, iv soaked up a load of knowledge.
I really appreciate you linking me to both of them and I will read them properly when I have more time.
I just wanted it put out there, I don’t get much money and so for me all these RXN’s are a very long drawn out thing by getting one reagent at a time because hardly anywhere sells things like 3,4,5-tmobza in quantities of less than 0.5-1kg!
Thats fine, it just makes things more drawn out as I don’t intend to sell anything…just the fact I could have as much mescaline as I’d ever want is a nice proposal ha
I am def learning a lot though - I would Never suggest I actually know my shit although I probably know JUST enough to make it sound like I do, I still couldn’t write my own synth so like after I make mescaline I wouldn’t then be able to make proscaline. Or just because I can follow and understand the DMT reductive amination doesn’t mean I understand how to balance the equation or make N,n-DET.
I think I missed the very basic part of chemistry where you learn to balance equations and learn how to utilise things I already have to modify it enough to have something else - If that makes sense!
One thing I did learn recently is that you can have private samples of whatever sent to labs in Spain for GCMS done on it. Would def do that….although for some things simple TLC is enough for me to trust in the chem

 

[The-Hive]

A lot easier way

DMT extraction using lye (sodium hydroxide) and naphtha

This article documents the procedure for one of the most common methods of extracting high-purity, crystallized DMT from one of its natural plant sources using a traditional acid-base (A/B) methodology.

m.psychonautwiki.org

 

[Rabidreject]

Haha yes has been done multiple times and yes is much cheaper and easier - to a point. I want to make enough N,n-DMT for the rest of my life and salt it out etc but I’d also like to explore other tryptamines like n,n-DET, DiPT, DPT of course - not saying I will actually get there with others than DMT but I’m confident I can get that done with the Chinese grade 99% purity tryptamine I have and a simple dry ice/ acetone bath instead of trying my luck with a simple ice bath.
But yeh acknowledged - if ALL you want to do is TRY DMT then sure an A/B extraction is for sure going to be easier but the better thing than the fact I may now be able to synthesise n,n-DMT (I think that’s cool in and of itself and quite unusual these days) is the fact it’s put me onto learning about organic chemistry and made me realise PEA’s and psychedelic amphetamines are much easier to produce than tryptamines!
I should have realised simply by the order in which shulgin wrote his books but nope, not that clever - I had a goal and was going for it lol
Now I have many goals with organic chem and am collecting all the time…chemistry has seriously opened my eyes to a world few ‘drug enthusiasts’ actually bother to learn. I mean shit - I been trying one psychedelic or another on and off for 20 odd years now - extracting DMT being a pretty large part of that but also buying lots of early (shulgins) RC’s in the early days, I’m amazed it’s taken me this long to actually REALLY dig into the subject tbf!
Anyone who is looking to make money (something I clearly am not) do NOT think it’s an easy guaranteed way of making money, I’d still just extract and re-x but still it is something I want to do!

 

[Rabidreject]

I just thought you guys should know where I’m coming from.
It’s actually pretty annoying not being able to think of other things!!

 

[Rabidreject]

Okay so does anyone have Ammonium acetate for sale?! Haha jk

 

[The-Hive]

EBay or ACP pure once you get the hang of chemistry, the drugs menu is your oyster, trust me I have tried about 90% of drugs, especially designer drugs

 

[Rabidreject]

Haha yer both of them have been fucking awesome for the most part - other than that a couple polish companies have been useful. A lot of the major chems I needed iv ended up just distilling from things already in the country though….
I need to finish that nitroethane synth I started actually. All I neeed to do is the final step now. I kind of forgot about it when I got a 150ml or so (minor atm - I am aware).
Anyway the next thing I need to work out is LiAlH4 as I can’t buy it pre-made. There are things I can buy from these companies (ordering to a flat) and things I def can’t. I was amazed I was able to find a company to deliver conc. Hcl acid tbf!

 

[Rabidreject]

I followed the mescaline / TMA video on here but was also keeping an eye on Pihkal.
I successfully made about 7-8g of the 3,4,5-b-nitrostyrene and so I thought I’d push my luck and try make the corresponding nitropropene as well.

So over the past few days I first did the reflux - then the next day I didn’t think the colour was right - according to shulgin so I refluxed it longer and this time in my mantle with a stir bar instead of in my steam bath.
I got the colour ‘better’ but not exactly as described so I let it cool overnight to RT.

Then next day I figured I’d do a vacuum distillation on it using my mantle. Can’t say I’d ever done one before.
I’ll admit I got some bumping at first, only once but hey - first time. After a while, however, I was left with a red oil.

So today after 3 days of doing stuff to this mad reaction, I decided to re-x the oil from MeOH, as per Shulgin’s synth.
I am now waiting for it to cool and I feel like it probably won’t work - I just seem to have REAL bad luck making nitropropene’s even though iv had great success with b-nitrostyrene’s and it’s the same reaction!
Very odd….

Anyway keep your for me!!

If I have any success I’ll share it.

I guess regardless, I still have two different b-nstyrene’s to reduce so that’s exciting on its own.

 

[Rabidreject]

Wow, got up this morning feeling pretty darn certain that the TMA synth had gone wrong and would crystallise.

Why? I have no idea really…maybe I checked it too quick but after abandoning it in the freezer overnight I was pretty darn surprised to see that it had been overcome by yellow crystals…
Score!
So now I have 6 or so grams of b-2,5-DMONS,
around 8 grams of un-recrystallised b-3,4,5-TMONS
then however much of the corresponding trimethoxynitropropene is in the following. I always mess the name of that nitropropene up for some reason. They don’t follow the same naming conventions as the nitrostyrene’s (from what iv seen them called in Pihkal anyway).

(Does this site always turn anyone else’s images 90 degrees as well?! It’s really annoying!!)

I will admit, i let it get too cold and it’s frozen solid but I’ll just pop it back in the fridge for a while before I filter.

To be honest, the same thing happened when I made the mescaline precursor - is why the photo I posted of it drying looked so wet. I just filtered, left it there for a while and by the time I put it into the weigh boat and then into the designator, it had melted and didn’t look any different from the 2,5-styrene.

Sorry for this long rambling post - I’m pretty happy to be honest as I really didn’t think it was going to crystallise this time!

It’s a really nice feeling just being able to actually follow one of Shulgin’s syntheses (or parts of) after having looked and read at this book for the past 20+ years on and off. Pretty much since the very beginning of the RC website era, when loads of Chinese sellers worked out they could sell most of them.
It’s just nice to follow his words and it work just the way he says.
I even actually followed parts of Shulgin’s write up’s over the video on here for this most recent TMA precursor. I like the way he includes things like - “I refluxed It until it was a nice dark red colour”.

To some degree, I actually find that description more useful than giving a reflux time. I mean, I did end up just checking it via TLC but still - if I hadn’t had access to that I would have carried on refluxing it longer as it was a deep yellow not even orange at the time so yeah it helped.

Anyway - iv been having FAR too much success in my ‘chemistry/alchemy’ recently so hopefully I won’t mess up the last step!