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PNP's into amphetamines reduction on alu foil
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brain
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re: PNP's into amphetamines reduction on alu foil

 Sun May 15, 2005 2:11 am		 Reply with quote
today "me friend" was doing 10 taimes this reaction, all day long ! so tired Smile ...

-he used as "alcohol" - denaturated alcohol (destilled) -not the best idea Smile but reaction was going... and product was obtained-and after puryfication-testet on IR-was preaty ~clean, but denaturated alcohols-can hawe differens substances in different countrys-toxic! -dont do it with this Smile -IPA-i think the best way, cheap, EtOH-goog but expensiwe way Smile

-he used as solvent (to extract amine) - Et2O-good, but expensiwe, and dangerous, the same results a had with xylene and naphta !! than i addes some IPA, and 98% H2SO4 , product was washed twice with acetone - the product had no smell ! [no naphtna or xylene smell] ...

-when adding NaOH to mixture-temp was helded at 20-30C [not more than 40C]

-the reactions was proceeded in baker ! widout reflux condenser

-not ewery time all p2np was reduced !! sometimes after extraction-extract was yellow, but i add to it H2SO4 directly, and onlu wash product with acetone ! pure product!

-Al foil grinded in electric mashine [for grinding sacharose or coffe] -was much better than cutted in 3x3 Smile

-the acid and alcohol was mixed ! then addes Al/Hg - when reaction starts, i added slowely P2NP crystals !! with good stirring Smile

BTW~the water is important! when destilled used-ewerything was good, when "normal" water used-not good Smile
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hAzzBEEn

Joined: 09 May 2005
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re: PNP's into amphetamines reduction on alu foil

 Mon May 16, 2005 10:26 pm		 Reply with quote
Earlier (much earlier) in this thread, IndoleAmine wrote:
Quote:
So: if you are dreaming about making methylated amphetamines, you should dream about making the P2P ketone intermediate with any method you like (reduction of nitropropenes with SnCl2, Fe/HCl, Fe/GAA etc; or a percarboxylic acid oxidation of propenylbenzenes like you described for example) and use Al/Hg to make methylamine "just in time" and condense that with your ketone (during the Al/Hg) to give final product.

Is it not possible to use Al/Hg to make amphetamine freebase, and then proceed to methylated amphetamines via Al/Hg with formaldehyde as per this quote:
Quote:
Formaldehyde and Aluminum Amalgam:
N-Methyl-amphetamines were prepared by the reaction of the corresponding amphetamine with formaldehyde and reduction in the absence of acid. Thus, a mixture of 1 mole amphetamine freebase (136g) and 1 mole aqueous formaldehyde (81ml 37% or 75ml 40%) in 350 ml alcohol and an excess of aluminum amalgam was reduced for several hours, water added, aluminum hydroxide filtered off, the solution acidified and evaporated, and the freebase separated by means of alkali yielding phenyl-N-methylisopropylamine, converted to the hydrochloride, mp 140°C

This is the link to the complete article:
https://www.synthetikal.com/Rhodiums_pdfs/chemistry/amphetamine.methylation.html

This may deserve it's own thread, but I thought it fit with the previous discussion.

EDIT: I started another thread at:
https://www.synthetikal.com/synthforum/about953.html
This thread is already long enough and has an established topic.
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brain
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re: PNP's into amphetamines reduction on alu foil

 Mon May 16, 2005 11:13 pm		 Reply with quote
it is posible-and simple-by the way Smile my friend is from 2 hours-proud poseser of ---- - "he" synthesied it from amph-freebase+HCHO--Al/Hg--> preaty easy ! Smile
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icecool
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re: PNP's into amphetamines reduction on alu foil

 Fri Sep 02, 2005 5:09 am		 Reply with quote
What would happen if you start steam distilling while the solvent is still in the Al/Hg reaction.
Quote:
And just for clarification of the whole process:
You are supposed to heat the post-rxn mixture in a distillation apparatus until all alcohol has been distilled away, then let cool down a bit and carefully add lots of NaOH solution, then apply heat again and steam distill out the amine together with H2O (add more H2O to the flask you are heating from time to time to comepnsate for losses), then basify the clean, water-like distillate you collected, and extract with a nonpolar (like ether) 2-3 times,


So if you would have basified everything including the solvent (EtOH in SWIM's case) and then start distilling it, normally as I read above it is so that one first needs to distill the EtOH off and THEN basify the mixture.
What would make the difference...
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icecool
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re: PNP's into amphetamines reduction on alu foil

 Sat Sep 03, 2005 4:20 am		 Reply with quote
Okay SWIM found out himself why it should be removed...
It doesn't per se needs to be removed before basyfying, but well it just needs to be removed.
Because: toluene, DCM, ether all dissolve in ethanol, so you can't extract your freebase...
You can steam distill directly out of the Al sludge but then you need to rotavap off the EtOH before you are able to extract it.
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