This article looks perfect! Dissolve your ketone (MDP2P, P2P or whatever) in alcohol and add to an acidified aqueous solution of an excess of your desired amine, then run 1.75V/50mA through the solution until the resistance of the solution has increased so much as the current drops to 5% of the initial value, then perform an acid/base wash and the crude amine (MDMA/MDE/Meth/whatever) freebase is isolated for vacuum distillation and/or HCl gassing.
The yield is 70-90%! Electricity is almost free, no soluble mercury salts are used, no watched, water-sensitive and/or expensive reducing agents and very little chemical waste.
1-(3-trifluoromethylphenyl)-2-propanone (2.02g, 10 mmol) was dissolved in a mixture of 10ml 70% aqueous ethylamine (150 mmol), 37.5ml 2M HCl and 50ml ethanol, the apparatus flushed with inert gas and electrolyzed at 10°C with a controlled potential of -1.75 Volt in a divided cell with a mercury pool as working electrode and a platinum anode. The current drops from an initial 50 mA to 2-3 mA when the necessary 1960 As has been consumed. Next the electrolyte is acidified to pH 1 by the addition of 2M HCl, the ethanol evaporated under reduced pressure, the aqueous phase washed with 2x50ml ether and 25% NaOH is then added until pH 14. The alkaline solution is extracted with 3x50ml ether, the combined organic extracts dried over MgSO4, filtered and the solvent evaporated in vacuo to give 2.0g (87%) N-ethyl-3-trifluoromethyl-amphetamine (Fenfluramine) freebase.
Synthesis 1005-1007 (1987)
https://www.thevespiary.org/rhodium/Rhodium/pdf/redamin.hg-cathode.pdf (https://www.thevespiary.org/rhodium/Rhodium/pdf/redamin.hg-cathode.pdf)
Thanks to Endo1 for bringing the article to my attention.
Looks like a good project for HiddenCloud. You will see...
Swim also got the idea from https://www.thevespiary.org/rhodium/Rhodium/chemistry/tcboe/chapter7.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/tcboe/chapter7.html)
on the section of electrochemical reduction from 3,4-methylenedioxyphenyl-2-nitropropene to mda freebase but that article goes mdp2p to mdma freebase..which is even better for hiddenCloud.
The cell hiddenCloud plans to work on is a divided cell but using graphite rods and a salt bridge instead.
Thanks chief...you will see soon HiddenCloud will have a writeup of electrochemical reduction to make honey :)
hcildoduedn
Hg is probably chosen for its hydrogen overvoltage. Maybe lead could substitute... oh, see Post 317018 (https://www.thevespiary.org/talk/index.php?topic=11557.msg31701800#msg31701800)
(PolytheneSam: "Condition/preparation of the lead cathode seems ...", Novel Discourse) and the whole thread and don't forget to UTFSE. I bet even ceramic cell divider has its increase in the resistance, no matter what.
I remember a while back that you mentioned that you have never read a detailed setup of one of these or seen such as have many. Here is the most detailed setup I have seen or read that may be of some use to you bees.
http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?rxntypeid=108&prep=CV6P0153 (http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?rxntypeid=108&prep=CV6P0153)
Yes, That pic really is me!
This article looks perfect! Dissolve your ketone (MDP2P, P2P or whatever) in alcohol and add to an acidified aqueous solution of an excess of your desired amine, then run 1.75V/50mA through the solution until the resistance of the solution has increased so much as the current drops to 5% of the initial value, then perform an acid/base wash and the crude amine (MDMA/MDE/Meth/whatever) freebase is isolated
That is so kool. The next thing I was going to ask in the newbie forum was 'why is P2P cool?', I was thinking about it a lot earlier today and last night.
So, can any of these "ketones" as you call them be transformed in to any of these "amines", or is there a specific initial ketone to correspond with a final amine?
Sorry if newbies aren't welcome in this forum!
True underground chemists take a ketone, do a reductive amination with it while crossing their fingers, after wishing for an end product and throwing a coin in the magical pond (there is only one correct pond so those guys really know their shit).
No. There is a reason why 1-(3,4-methylenedioxyphenyl)-2-propanone (MDP2P) yields 1-(3,4-methylenedioxyphenyl)-2-methylaminopropane (MDMA) after reductive amination with methylamine. If you draw these three molecules on a paper side by side you can understand. Alternatively you can take a look at https://www.thevespiary.org/rhodium/Rhodium/chemistry/mda.dalcason.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/mda.dalcason.html)
.
And you are right about the newbee forum thingie. This post belongs there as well. ;D