Síntese da dextroanfetamina (Nabenhauer, 1942)

[G.Patton]

Preparar uma solução de ácido sulfúrico em acetona numa proporção volumétrica de 1:10. (с)
Tomar 1 volume de ácido e 10 volumes de acetona

Não há problema. O objetivo é atingir o pH= 11-12, pelo que a concentração não é tão importante.

 

[Morgan prothero]

Will this work? How important are measurements this blows my mind seems very straight forward

 

[G.Patton]

Please, ask more precisely what do you mean. I don't understand your question.

 

[waltjr5858]

I have tried the AL/HG a couple times with no success yet... typically the product separates from the sludge looking pink to red with no activity whatsoever. I'd like to try the dripping in idea but how are you keeping the aluminum from becoming non reactive as it sits there in air. I see you call to drop 30mls of water in but that won't cover the aluminum that is amalgamated and it doesn't take long for it to become unreactive. I have had this happen and the reaction just flat out stops. How are you keeping the reaction going?

 

[G.Patton]

That is typical result of overoxidation and overheating during acidification procedure.

You can don't wash your Al/Hg by water and carry out reaction directly there.

 

[waltjr5858]

It's not the product that was pink or red it's the alcohol solution after adding the base waiting for layers to separate.

 

[waltjr5858]

So just to double check because I'm going to try this way due to severe inconsistency the regular way.after the aluminum is amalgamated it gets rinsed right? At that point what do you do to keep the amalgam from being oxidized? Your instructions say to add water before dripping but that small amount doesn't sem like enough to keep the aluminum covered to prevent oxidation and the aluminum from becoming inactive. After rinsing out the mercury what do we fully cover the aluminum with to keep it ready to react?

 

[G.Patton]

As I already said, you can not rinse it and continue reaction right there on Al/Hg. Do you understand right now?

 

[waltjr5858]

Ok I will try that too but in the original instructions put up how is that kept from oxidation? And now if not rising when using 2g to 20ml of nitric acid to make Merc ii nitrate what ratio of that to aluminum is used? Too much and it eats the Al fast and too little and nothing happens? Doing it this way when is the right time to start dripping?

 

[Chemdogkm]

what is the purpose of adding nickel chloride hydrate to this reaction ? A second catalyst?how does it work and should it be used?

 

[G.Patton]

It is not necessary.

 

[Chemdogkm]

is it a substitute for aluminum?

 

[Chemdogkm]

can it be used and how so? I see it is mentoined in multiple synths

 

[Chemdogkm]

sorry to bother,im sure playing 20 questions gets old

 

[Rabidreject]

As for MDA synth, I hate to disappoint but I bought the md-p2np already made - I don’t like the group of drugs enough to bother doing the Henry reaction etc but seeing as I saw it for sale, I reduced some over the previous couple days (via NaBH4 catalysed by copper - although from my understanding there are many ways to reduce nitroalkene’s) and now I have a bunch of r-MDA.
Now I will follow the latter part of the synthesis from where you have your r-amphetamine.
I can’t say I have ever seen 3,4-MDbenzaldehyde for sale…I take it that is the same as piperonal?

 

[Chemdogkm]

mda turn out good?

 

[Rabidreject]

Yes fantastic actually.
77.9% yield! Real clean looking crystals too

I can’t say iv tested it yet though, methylenedioxy compounds aren’t really my thing but I will do at some point…

 

[Eleusius_hive_reboot]

hey patton !


i HATE Hg-Salts......

(who doesnt ?) I MANAGED TO SUBSTITUTE THE AGENT; to break the oxide layer, by catalyst poisoning,


YOU CAN USE SEVERAL OTHERS LIKE:

1. Gallinstan (known in newer lit. already, but a bit trickyer...)

2. Tetrachloroaurate with zinc-copper coupling complex.

===== BUT NOW, LADIES AND GERMS ============

PRE TREAT THE ALUMINUM CUTTINGS WITH ULTRA SONICATION BATH

(CREDITS TO ARTIFFICCIAL INTELLIGENCE FOR SCIENTIFIC PURPOSES)

this f**king DID THE JOB !!!!!


tried it for p2p -> imine reduction......its comparable to my former NaBH4 dreams...!

 

[G.Patton]

It would be nice to see your detailed tutorial in a separate topic (with pic would be cool if it's possible).