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Laboratory Tips Safety proceedures, test reagents, drilling rubber stoppers, bending glass tubes, etc. Contributed to by chemists.

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  #1   Add cbb2k to your ignore list  
Old 2003-06-29, 21:19
cbb2k cbb2k is offline
 
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Hello,

SWIM is interested in the hydrogenation

via PD technique.

SWIM's question is, does the ammount being

used need to - Weigh - so much?

Fester referenced PD plating on a screen,

which tells SWIM the ammount might not be

as important as the surface area of the

piece?

SWIM has a piece of palladium 1" x 1" aprox

1/16th thick, about 2.5 grams.

1" x 1" equals roughly the surface area

referenced in festers paper.

So, Should SWIM be able to continue

experimenting with the formula, or

would it be an incomplete reaction,

and result in the starting material

being unchanged?

Thanks.

[Edit: Spacing]

[This message has been edited by cbb2k (edited 06-29-2003).]
  #2   Add cbb2k to your ignore list  
Old 2003-06-30, 10:18
cbb2k cbb2k is offline
 
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bump
  #3   Add stochiometria to your ignore list  
Old 2003-07-03, 07:56
stochiometria stochiometria is offline
 
Karpatia
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Forget it. UFs electro never worked in reality - only variations which used additional palladium catalyst yielded some product which was meth and not chloroephedrine or a ester of ephedrine which has to be prepared to get anything going. This ended up in a catalytic hydrogenation with palladium on charcoal (Pd/C) with electrolytically produced hydrogen.....

There are more drawbacks. Forget it.

Unbelievable amounts of time and money have been wasted on this - spare your Pd for something better and use HI or the Birch. Both are perfect methods for this reduction, high yielding and low effort compared with electro, Pd/C or Pd/BaSO4.

Catalytic hydrogenation would work like this: Solvent: GAA (glacial acetic acid)

Catalyst: Pd/BaSO4 (palladium disposed on bariumsulfate)

Activator: perchloric acid

Hydrogen: fuel cell grade (forget homemade or welding)

All solvents degassed and ultraclean to avoid poisoning of the catalyst. Pressurizing the vessel to 3 bar, shaking not stirring, perchloric 70% is added to activate. Ephedrine/pseudo is used as hydrochlorid (freebase should work also). Temperature max. 80°C - better 60°C or lower.

Time: 1 hour to 16 hours (pressure, catalyst, temperature...)

.....

favorites for realworld:

- for the McGyvers: Sodium Birch

- for the rural ones: Birch with Li from batteries

- for the Worlockian traditionalists: hot and dry cook for mindspoil meth. (hello AM! Here are you by! huhu!!)

- for those who want it more relaxed in reaction and product: HI prepared in advance. Some RP/H3PO2/H3PO3 + pseudo + refluxed for 4 to 12 hours (Some iodine handy for adding it if seems necessary). If enough HI is used from start, the RP etc. isn´t needed at all.

10 gram pseudo and 25 ml HI 57%. Four hours reflux = Meth. (thanks to Hematite) Substituting water by acetic acid is ok - if reaction like above won´t get going add 10 ml GAA and 2 gram RP (2 ml H3PO2, 3 ml H3PO3), iodine by thumb. The problems are in this case not on the method but on the pseudo and Gakk. Often the GAA alone is enough already.

Clean the fucking pills - thats hard nowadays, what looks clean isn´t clean mostly.

Make HI in advance.

Get gogo.

Actually it isn´t so hard.

StOcHioMeTRiA !

  #4   Add NeverSleepy to your ignore list  
Old 2003-07-03, 08:18
NeverSleepy NeverSleepy is offline
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mindspoil would be a great nick for one who advocates dry rxns

teehee
  #5   Add stochiometria to your ignore list  
Old 2003-07-07, 02:18
stochiometria stochiometria is offline
 
Karpatia
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It seems nobody has interest in a conveniant way to produce this highly desired substance "methamphetamine" or "N,(alpha)-Di-methylbenzeneethanamine" (don´t know how chemists can stand this, LOL...).

You need to make some hydriodic acid in advance - whats easier as doing it in the reaction with pseudo and much better controlable.

How to make HI?

- from red phosphorus and iodine in water and/or acetic acid

- from sodiumiodide or potassiumiodide and phosphoric acid

just to name the most common ways.

Hey! no more matchboxes and tincture! A visit at the hydroponics store and the swimmingpool supply and your needs are done for a long time!
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