MDP2NP to MDA via NaBH4/CuCl2 reductive amination?

InLikeFlynn

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Is it really as simple as substituting P2NP with MDP2NP from the one-pot synthesis sticky for amphetamine? What other considerations should I have if this does work?
 

Pulser

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1. you will require MDP2P/ammonia acetate >imine> to produce MDA.

2. if you have NaBH4, no need for CuCl2.
cyanoBorohydride works better in this reaction.
 

InLikeFlynn

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Unfortunately no access to MDP2P (unless I am able to convert the MDP2NP into MDP2P) or cyanoborohydride. I do have access to NaBH4/CuCl2 from other nitrostyrene experiments and MDP2NP.

The method I am referring to in the original post is here: https://bbgate.com/threads/one-pot-amphetamine-synthesis-from-p2np-with-nabh4-cucl2-1kg-scale.70/

I was just curious if MDP2NP can be substituted for P2NP, would the methylenedioxy group survive the reaction and similarly to P2NP and produce MDA?

I'm reading some success reducing MDP2NP to MDA in this thread here: https://www.thevespiary.org/talk/index.php?topic=15090.0

But I was wondering if anyone had done it and had any first hand experience or tips for the synth, if it is possible.
 

Pulser

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Must of been a real late night for me, to answer a totally different question to the one you asked.

I'll look into it for you and see what my opinion is.
 

Jordan Belfort

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If you do a Al/Hg, Al/Ga with iodine (else it doesn't work) and heating till 30-35 celcius, and you replace methylamine/nitromethane with ethylamine/nitroETHANE it will also work in a one pot.
 

Melv99

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Yes it works exactly the same. Result is Mda instead of just A. Would suggest distilling off IPA, adding base and extracting with a NP. Then normal work up
 

InLikeFlynn

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Are there many physical property differences between MDA Hydrochloride and MDA Sulphate? I’ve never set up an HCl gas apparatus before and want to just try to salt with sulphuric acid out of laziness, unless it really is worth it to do HCl, then I’ll go ahead and learn lol.
 

InLikeFlynn

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I’ll report back when I try this synth. Will probably be my next project :)
 

Melv99

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Do the sulfate as usual. It’s easier if you already know the procedure and you’ll know if you actually produced anything. You can try Hcl later then you get the hang of it if you want.

Sulfate seems to be better choice all around for MDa….. or so I’ve read.
 

Akashic

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Since it happens to be relevant to current evolution of the post, how come mda hcl doesn’t have the same hydroscopic properties as amp hcl?

As for the reduction, I’ve been wondering big time about this myself… if it really works as direct reducer of that respective nitrop, the nabh4/cupric would byfar be the clandestine route. accessiblity LiAlH is limited and expense or with amalgam you got the mercury to contend with, why risk it if you don’t have to.

also I think sulphate whatever sucks personally, and weaker than respective hcl salt. Where’s someone who really knows what they talking about how do we get the stable amp hcl, No goo puddles
@InLikeFlynn hypothetically Practice that hcl generation make yourself a decent apparatus ex drip funnel,one hole stopper, filter flask, ptfe hose off the nipple, in line drying tube glass tube tip and clamp it on stand. Without additional drying I’d go with dripping sulfuric on aqueous hcl and nacl wet slush consistency. And do some dry runs before you attempt on the precious hypothetical fb you worked for
alternatively, titrate w/ aqueous Hcl 37% I believe is actually the best however takes more skill. hypothetical you must accurately add x amount of acid down 6 to 5.8 trick is in the addition it’s only added once and left to xtal without disturbance
 

HerrHaber

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I had this prepared with no inconvenience I can remember of, my means of Al/Hg reduction but can't remember what acid is involved I isolated the actual salt but the salt form is suitable for longer term storage and not needed if you plan to methylate the nitrogen (which I never did).
 
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