In post
Post 335851 (https://www.thevespiary.org/talk/index.php?topic=12127.msg33585100#msg33585100)
(Sunlight: "MDA and MDMA from CTH reductive amination", Novel Discourse)Sunlight says this:
In conclusion, the rxn works as claimed in the reference for MDP2P and probably with other interesting ketones, and yields will depend on the amount and activity of the catalyst. Probably a 20 % weight from ketone of a good catalyst is enough to get the best yields.
2 gr ketone, 6.9 gr AF in 33 ml of 1:10 solution, added 1.35 gr of 10 % Pd/C (second time used), stirred 16 hours, 81 %. (Pd/C similar to reference)
That is almost 20% Palladium w/w to the ketone and then it is going to be an expensive hobby.
So what does he mean. 20% w/w 10% Pd/C or so much catalyst that the Palladium is 20% w/w with the ketone?
That is almost 20% Palladium w/w to the ketone and then it is going to be an expensive hobby.
The Pd/C is reusable.
If SWIM want's to do a 1 Kilo batch he needs Catalyst with 200 grams of Palladium. That costs 1000 Euro's and if he reuses that damn stuff 5 times it still is expensive.
If this works with 20% w/w 10% Pd/C then a 1 Kilo batch the Palladium only costs 100 Euro's. God that is a fucking difference. Especially when he reuses that catalyst 5 times.
Do this reaction works like claimed with 20% w/w 10% Pd/C?? Economics is everything and Palladium isn't getting cheaper. Only more expensive.
It seems like a much higher catalyst load is needed when MDA is synthesized, compared to MDMA. When MDMA is the desired product, the catalyst load is a lot less:
When we tought time ago about a similar rxn to this one, we thought as well in making MDMA. We added a bit of aq methylamine and formic acid to methanol, and then a bit of Pd/C and we observed a clear decomposition of the formate, so we tried the rxn with aq methylamine and formic acid and TLC was very good, then we make a test with 3 gr:
3 gr of ketone, 4.4 ml of 40% methylamine, 2.4 ml of 98% formic acid in 30 ml of methanol, 300 mg of 10% Pd/C stirred 48 hours, 83% yield.
And Urushibara. If I use an Overload amount of Urushibara would it work equally good as Pd/C for MDA?
I have never heard of any Urushibara CTH being tried out.
Ok. Raney Nickel. Would Raney Nickel work?
And normal hydrogenation?
i think it is high time some enterprising bee triied out Urushibara catalysts with a CTH. In fact Ab2 clearly remembers seeing a reference for a Ni catalyzed CTH with formic acid as the hydrogen donor, it might have been posted by jim like two years ago or so
In this paper
Reductive Amination Review (https://www.thevespiary.org/rhodium/Rhodium/chemistry/reductive.amination.html)
(https://www.thevespiary.org/rhodium/Rhodium/chemistry/reductive.amination.html) They make Amphetamine from P2P. Amphetamine is almost like MDA. Only that MD groep is different.
In that paper Pd/C or Pt catalyst also doesn't do a very good job. Raney Nickel produces High Yields At low pressure in this paper so
maybe Raney Nickel is the way to go. At least it sounds logickel. ::)
because it's activity is W-4 and the equilibrium between ketone/imine/and amino carbinol is to the left