Sunlight's CTH MDA

[flipper]

In post

Post 335851

(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?

[Rhodium]

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.

[flipper]

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.

[Rhodium]

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.

[flipper]

And Urushibara. If I use an Overload amount of Urushibara would it work equally good as Pd/C for MDA?

[Rhodium]

I have never heard of any Urushibara CTH being tried out.

[flipper]

Ok. Raney Nickel. Would Raney Nickel work?
And normal hydrogenation?

[Antibody2]

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

[SPISSHAK]

[flipper]

In this paper

Reductive Amination Review

(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.  

[SPISSHAK]

because it's activity is W-4 and the equilibrium between ketone/imine/and amino carbinol is to the left