11-06-03 15:00
No 469121
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?
(Chief Bee)
11-06-03 15:34
No 469127
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.
(Hive Bee)
11-06-03 17:51
No 469163
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.
(Chief Bee)
11-06-03 18:37
No 469169
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.
(Hive Bee)
11-09-03 11:55
No 469775
And Urushibara. If I use an Overload amount of Urushibara would it work equally good as Pd/C for MDA?
(Chief Bee)
11-09-03 17:56
No 469802
I have never heard of any Urushibara CTH being tried out.
(Hive Bee)
11-09-03 18:08
No 469804
Ok. Raney Nickel. Would Raney Nickel work?
And normal hydrogenation?
(Hive Addict)
11-09-03 22:19
No 469832
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
We are all just witnesses.
11-11-03 02:41
(Rated as: no sources!)
(Hive Bee)
11-11-03 07:01
No 470114
In this paper Reductive Amination Review (../rhodium /reduct
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.
(Hive Addict)
11-11-03 07:34
No 470120
because it's activity is W-4 and the equilibrium between ketone/imine/and amino carbinol is to the left