Practicing on mesc.

[PEYOTE]

Hi!

SWIP wanna make some mescaline for AFOAF. So he had decided to try this route:

1) Vanillin =(I2/NaI)=> 5-Iodovanillin =(Cu/NaOH)=> 5-hydroxyvanillin (*)
2) 5-hydroxyvanillin =(MeI)=> 3,4,5-TMBA
3) 3,4,5-TMBA + MeNO2 =(AcONH4)=> 3,4,5-TM-b-NStyr
4) 3,4,5-TM-b-NStyr =(some reductant)=> M!

(*) ref is:  

https://www.thevespiary.org/rhodium/Rhodium/chemistry/iodovanillin.html

For the nitromethane, he wanna make it from MeI and NaNO2. That's obviously possible, but in practice? There is some refs for this simple reaction? Conditions, solvent and so on?

Then, another Q: Is it possible to store 3,4,5-TM-b-NStyr indefinitely or does it degrade after a while?

Thanks in advance.

 

"Dark star crashes, pouring its light into ashes..."

[yellium]

The cheapest (and easiest) way to get mescaline is buy some san pedro, and extract the good stuff out of it. UTFSE, and you'll find that the vanillin->3,4,5-TMBA->mescaline route isn't exactly easy; especially if you don't have access to basic chemicals and chemical equipment.

[PEYOTE]

He has access to almost 18.000 chemicals products and almost any type of equipment (even if SWIP's a bit worried about his cash disposability), so that way is for SWIP feasible.

"Dark star crashes, pouring its light into ashes..."

[bujinkan]

arent yeild rediculously low for san pedro extractions?
I say things just to see how they sound=) 

[yellium]

If you have access to 18.000 different chemicals, why do you bother making your own nitromethane, and are you still uncertain about how to do the reduction of your nitrostyrene?

Regarding yield of san pedro extractions: I've never performed an actual extraction, so I can't say anything about yields.

[Rhodium]

Yellium: Probably because he, like myself, reside in Europe, where it is ridiculously easy to get an account with most chemical supply companies, even if you are still an undergraduate student.

I agree that it is more expensive to make your own nitromethane than buying it yourself though. It is not watched or anything, it is even available OTC.

[PEYOTE]

Yes, SWIP has access to that number of chemicals, but for example nitromethane is quite expensive on that database, and SWIP thinks methyl iodide, used for methylation, can be used for producing nitromethane too, cause NaNO2 is very cheap, do u understand? It's only a question of price! On the other hand, SWIP could buy 3,4,5-TMBa ready to use, but the seller could understand for waht purpose SWIP'll use it...
"Dark star crashes, pouring its light into ashes..."

[Rhodium]

The yields of MeNO2 from MeI isn't brilliant, for all practical purposes it is better to buy ready-made MeNO2. If your particular supplier is expensive, search for another one. Nitromethane is sold as model car racing fuel in europe too, go to your nearest model car shop and ask for it - they will at least have methanol/nitromethane mixtures for sale, which you can distill. Do not buy 3,4,5-TMB from chemsuppliers directly, that is asking for trouble.

[PEYOTE]

Well, you're right, Chief, SWIP'll buy nitromethane. But it is also to make some practice that SWIP wanna make MeNO2 at home. And for the rest of the steps? Is all ok? Is 3,4,5-TM-b-NStyr stable? This is only SWIP curiosity...

Ah, thanks a lot for changing my title!



"Dark star crashes, pouring its light into ashes..."

[yellium]

You could also try the acetonitrile route, which does not need nitromethane. See escaline (PiHKAL #72) for details. PiHKAL #119 might also be interesting.

[Osmium]

So you think nitromethane is expensive, but MeI is dirt cheap? I don't know what supplier you intend to use, but that surely must be a strange company that is selling MeI for less money than nitromethane. Did you realise that the molecular weight of I is about 120g/mol?
Besides, as everyone else said, MeNO2 is OTC.
I'm not fat just horizontally disproportionate.

[PEYOTE]

...with MeI I pick up two pidgeon with one favus. (hoping this is the right translation....). But these are only waste-time discussions....

"Dark star crashes, pouring its light into ashes..."

[yellium]

No they're not. MeI is carcinogenic, and making nitromethane isn't exactly a piece of cake (actually, it is; it is only the separation and isolation of nitro(m)ethane which is a major pain in the ass.)
 
It is also very likely that you'll end up with something which smells and looks like nitromethane, but you don't know its purity. So you might be wasting valuable precursors.  Again, UTFSE. And ask yourself why someone would add IPA to some aldehyde+nitromethane, when you can buy 15% nitromethane in methanol?

[Rhodium]

3,4,5-Trimethoxynitrostyrene is stable if recrystallized and pure (canary-yellow). Store away from heat.

[hest]

Yep. I'm sure ther is a lot of info on M at the hive.
Just follow the synth at pikhal (or the on by rhodium with KF, yeald damm high) the LAH red. is not that greath 60-70%

[yellium]

IIRC, the formation of the nitrostyrene isn't that high-yielding also. I've heard that the nitrostyrene from M
is relatively soluble in methanol, so if you follow PiHKAL to the letter, you'll loose a lot in the (re)crystallization of the nitrostyrene.

[hest]

Iff you fress the methanol, ther won't bee much styrene back in it. (I'v once evaporated the methanol after the rex. and is was just 2-5%(of the nitrostyren) goo)

[terbium]

Post 276557 (missing)

(terbium: "Re: Mescaline synthesis questions", Newbee Forum)