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All 11 posts Subject: Sunlight's CTH MDA Please login to post Down

flipper
(Hive Bee)
11-06-03 14:00
No 469121
      Sunlight's CTH MDA

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
(Chief Bee)
11-06-03 14:34
No 469127
User Picture       The Pd/C is reusable.

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
(Hive Bee)
11-06-03 16:51
No 469163
      If SWIM want's to do a 1 Kilo batch he needs...

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
(Chief Bee)
11-06-03 17:37
No 469169
User Picture       MDMA vs. MDA

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
(Hive Bee)
11-09-03 10:55
No 469775
      And Urushibara. If I use an Overload amount of

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

Rhodium
(Chief Bee)
11-09-03 16:56
No 469802
User Picture       I have never heard of any Urushibara CTH being

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

flipper
(Hive Bee)
11-09-03 17:08
No 469804
      Ok. Raney Nickel. Would Raney Nickel work?

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

Antibody2
(Hive Addict)
11-09-03 21:19
No 469832
      don't give up so easy

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.

SPISSHAK
11-11-03 01:41
      try this on for size!!!
(Rated as: no sources!)

flipper
(Hive Bee)
11-11-03 06:01
No 470114
      In this paper Reductive Amination Review They...

In this paper Reductive Amination Review (https://www.rhodium.ws/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. crazy

SPISSHAK
(Hive Addict)
11-11-03 06:34
No 470120
      the reduction works with nickel

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

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	All 11 posts		Subject: Sunlight's CTH MDA		Please login to post		Down


		flipper (Hive Bee) 11-06-03 14:00 No 469121				Sunlight's CTH MDA
						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 (Chief Bee) 11-06-03 14:34 No 469127				The Pd/C is reusable.
						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 (Hive Bee) 11-06-03 16:51 No 469163				If SWIM want's to do a 1 Kilo batch he needs...
						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 (Chief Bee) 11-06-03 17:37 No 469169				MDMA vs. MDA
						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 (Hive Bee) 11-09-03 10:55 No 469775				And Urushibara. If I use an Overload amount of
						And Urushibara. If I use an Overload amount of Urushibara would it work equally good as Pd/C for MDA?



		Rhodium (Chief Bee) 11-09-03 16:56 No 469802				I have never heard of any Urushibara CTH being
						I have never heard of any Urushibara CTH being tried out.



		flipper (Hive Bee) 11-09-03 17:08 No 469804				Ok. Raney Nickel. Would Raney Nickel work?
						Ok. Raney Nickel. Would Raney Nickel work? And normal hydrogenation?



		Antibody2 (Hive Addict) 11-09-03 21:19 No 469832				don't give up so easy
						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.



		SPISSHAK 11-11-03 01:41				try this on for size!!! (Rated as: no sources!)



		flipper (Hive Bee) 11-11-03 06:01 No 470114				In this paper Reductive Amination Review They...
						In this paper Reductive Amination Review (https://www.rhodium.ws/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 (Hive Addict) 11-11-03 06:34 No 470120				the reduction works with nickel
						because it's activity is W-4 and the equilibrium between ketone/imine/and amino carbinol is to the left

All 11 posts	End of thread	Top