High yielding trans-2,5-Dimethoxy-beta-nitrostyrene synthesis (detailed description)

Swirly

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2c-e also does not seem difficult in the end:

You've already learned the Henry reaction, now do the NaBH4+ Cu(II)Cl reduction and all will fall into place.

Oh and there was even some 4-ethyl-2,5-dimethoxynitrostyrene sold on etsy recently albeit a tad pricey. Can't find it now.
 

Rabidreject

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Etsy is a mad one like that - my best supplier I found through Etsy. In fact the person that enabled me to do most of this chemistry I met through Etsy.
I just forget to search it regularly - I too have def seen relevant nitrostyrenes on there but as you say was expensive and I figured I needed the practice of getting the aldehyde all the way to the phenethylamine.
Don’t know why - there was just something in me wanting to see these incredible bright coloured needle crystals grow…it really is quite incredible. Especially having come from a reaction that I was having trouble getting to crystallise (DMT).
 

Rabidreject

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Oh and yeah I do intend to start with the CuCl2 + NaBH4 method…
 

Rabidreject

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Okay so I don’t have a rotovap and the synthesis said to remove the excess solvent under vacuum and so the only option I really have atm was just a normal vacuum distillation.
So I set it up using my mantle and rotary vane pump.
Im left with a dark amber/ red oil (I imagine also some residual nitromethane). I shall try to make it crystallise with temperature modifications but if it refuses to grow any crystals I guess ill have to re-x the oil from something - this is the TMA Henry reaction I am trying here as I had good success with the nitrostyrene version of the same reaction.

As I said, I essentially followed the video on here for mescaline/TMA whilst also reading Shulgin’s write-up’s as he mentions things like colour etc. I think he may have been left with an oil in this synth as well but honestly iv read so many different Henry reactions in the past few weeks I think my head is a little overloaded with such similar stuff.

I should really just try a synthesis from start to finish but I never seem to manage that!
I realised earlier that I already have two nitrostyrene’s to reduce - if this TMA synth does work for me and I get crystallisation of the nitropropene then when I come to reduce them all, I’m going to have lots of things to try…bit of a silly way of doing things really but hey ho!

Oh also I weighed the dry, crude b-3,4,5-TMONS and I think it was around 8g.
I know that probably seems really inaccurate and an estimate and to some degree it is coz I weighed it this morning…I dropped again on my meds a couple days ago so my heads pretty foggy.

Anyway thanks for all the help and suggestions - I’m going to start trundling onwards with the reductions now I think.

I have essentially been waiting for around 20-25 years to try mescaline and first bought a mescaline producing cactus around then. I now have so many huge different Trichocerius species - I don’t much fancy chopping up 20+ year old, beautiful cacti when you can just order an aldehyde from bloody china!
Also from my understanding a lot of the sickness with mescaline comes from the plant matter people don’t get rid of properly or just eat the cactus flesh itself.

Either way, I’m a big baby about feeling sick so iv never gotten round to it…

Now I am just one step away - okay well, two or three depending on how much re-x’ing I have to do.

It would be nice to have that one nitropropene though; I must admit.

I seem to have issues making nitropropene’s so I’m guessing the nitroethane I can obtain, isn’t as good or pure after distillation as the nitromethane mix I buy.

I really would like a rotovap, I must admit.

I was surprised how high I had to put my mantle just now when I was doing a vacuum distillation.
The vacuum was held at 0.9 bar, temperature was 40c on the distillation thermometer and just above that on the one in the actual RM.
I was just surprised at how high I had to have my mantle, even though the temperature was low inside the flask.

That was the first vacuum distillation I have done and I shut it off just as it was getting close to 70c purely because the guy in the synthesis set his rotovap bath to 82 and so I figured I didn’t want to heat it too much…

It really annoys me when I see people who use a rotovap to extract things to use in their ‘mixology’ making alcoholic drinks.
I see people like that on YouTube and although I appreciate using tools for things they aren’t really made for, I’m not ashamed to admit I’m just jealous of them!

I know people say you don’t need one unless you have a certain amount of output but still, it would cut down on ordering solvents - which is fairly important for a ‘clandestine’ lab. (Not that I’d really call my place a lab but I guess it is in a loose sense of the word!)

Certainly in the sense of things like DCM, which I’m not really allowed - it just cuts down on danger.

Honestly though I think I’d use one for reducing reaction mixtures and re-x’s. Getting things to crash out without being exposed to a load of air. Vacuum distillations are a bit of an ass compared to simple pouring whatever you have into a flask and switching a device on!
 

Rabidreject

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Oh wow. It’s quite incredible how the viscosity changes inside the flask, even after the outside feel completely cold.
I just left it on top of the fridge like ten mins ago and it swirled around the flask no problem, which is why I said there’s still nitroethane in there.
Im sure there still it but I’m guessing it’s less than I first thought because it’s a thick oil like THC or something now…

i just stopped and looked this up in Pihkal - turns out when he synthesised it this way, he also obtained a red oil after removal of solvent under vacuum.

I guess iv followed his write up so far, so I may as well continue!

Oh good I’m pleased about reading that actually, I thought I had over heated it upon solvent removal but I probably just about got away with it. I will admit I got some bumping at the beginning but overall I guess it did the job - it’s just annoying. I can TOTALLY see why people use short path more so than normal vacuum distilling tbh even if it’s not really what it’s for….
 

Rabidreject

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Oh also regarding crystallisation of DMT from tryptamine via reductive animation at cool temps, I have found that once I have the crude DCM mix; the quicker I go ahead and remove the solvent and then re-x, the better crystallisation I get.
No idea why, I also have to use a fuck ton of heptane (compared to any other re-x iv ever done).
Also I find it odd and off putting that the original yellow oil that you are re-x’ing doesn’t actually mix with the boiling heptane. It’s just a super weird re-crystallisation in general!
I need to try it with actual dry ice at some point - some people say it really helps some people say you don’t need it.

I think a little of both. You do get product but my yields were awful!!

Iv just had way better luck with phenethylsmines all round so far!
Mind you, saying that iv yet to actually make an active phenethylamine substance and iv met the gods with just a tiny amount of the DMT I made so I guess it’s a matter of opinion which is better lol I just mean iv generally had much better luck with the first step. I’m about to try the second step in a bit when I get home! It annoyingly also involves pulling off the solvent under vacuum (I guess I could evaporate the DCM but I had good success last time I removed that nitroethane…)

by the way, if you need any 3,4,5-TMOBA so that you don’t have to buy half a kilo of a kilo I’d be happy to sell you some. It’s getting the nitro that’s annoying though. NitroEthane is okay you can get from RS industries in their acrylic extruding binder product but nitromethane that isn’t with methanol is super annoying to find! It stinks to distill as well, that nitro fuel. In my experience at least. Someone gave me a great idea which was to add water to it, the only thing is with mine it also pulled the oils and the dye’s with it in the nitro layer! Still…a good idea, I thought!

Bt if a ramble sorry!
 

Rabidreject

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Oh and yes I tried using one of them aspiration’s from china and it was shit! Couldn’t connect it to my tap well at all!
Connected it to my water pump and (fart sound)!
 

Rabidreject

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One more thing re-pumps. I’m pretty amazed mine does still work as I added the total wrong oil to it!

I’d lost the manual that came with it, bought this vacuum pump oil and when it came it was orange lol

so I filled her up and I noticed when I turned it on it smelled like a garage with cars being fixed. I then found the manual and drained the oil and replaced with the correct iso value!

My pump was just from Amazon when I bought a vacuum chamber to turn into a desiccation! I was actually really impressed by the vacuum it pulled when I did a Vac Dist.
It remains to be a pain in the asshole to setup and run tho! I’m saving for a rotovap but I realised I needed a water circulating pump to be able to pull a vacuum without as much noise! Also I believe it will run my coolant for me too which is cool.
I also have a short path distillation head now so that may come in handier to be able to remove solvent, I dunno - certainly easier to setup than a full distillation set.

It is something I’m going to need to do more and more now, unless I want to waste a really hard to obtain solvent/reagent. Gah!😩

You read pihkal and just think I wish I could just pickup a phone and order pure nitromethane or nitroethane! I believe it’s because of all this separating OTC mixtures which is why I’m super sick of distilling stuff!
 

arundo

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I'm not sure but I believe that I read this report somewhere years ago.
 

Rabidreject

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Could be, someone else mentioned using a superglue as a catalyst for both the 3,4,5-TMOBA condensation reaction as well as the 2,5-DMOBA one, that sounded interesting, mainly coz I’m working with 3,4,5 atm and anything I can do to reduce my use of NM would be good. Hang on let me look in my messages….
 

arundo

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I'm referring the OP.
 
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