SHAKE AND BAKE INFO

[Niceiceinn]

HI Im new here but not on the block.

please fill inn what I can not seam to remember

efedarin / psudo
what you need is
ammonium hydroxide
sodium hydroxide
some Lithium
Ether
Dry HCI gas

am I forgetting anything here

thats it its all I remember can anybodi help me with this?

 

[MadHatter]

Ammonium Nitrate, not hydroxide.

 

[Niceiceinn]

my bad,I was just recolling it from my ADHD memmory hehe

 

[G&A3007]

MADHATTER....
can you use ammonium chloride/sulfate for shake n bake,
or only nitrate...
I could imagine the HCL side of NH4CL would or could stop LYE from turning the PSE to a freebase hence dis-allowing the PSE into the solvent to be reduced....
however im only looking at it from a glance, can you please confirm for me....thanx

bmk007

 

[Bartholomeus]

Stop producing shake and bake dope and get some proper glassware, you can thank me later

 

[MadHatter]

I second this. Ths is a trailer trash last-line-of -defence mthod. C'mon, glassware is freely available on Ebay. Check out Nanshinglass or Deschem. Not that expensive either.

 

[Sascha]

HI Im new here but not on the block.
Ok so first of all, the term shake and bake is more like the awful American redneck variation of an elegant Birch-Reduction.


Sascha’s Birch Reduction using Lithium, reducing (R/S+) Ephedrine to methylamphetamine.

Needed:

• 99% isopropanol alcohol
• Lithium
• Ammonium Chloride ( pure )
• Acetone ( pure )
• Dry ice
• Sodium Hydroxide ( NaOH >99% )
• (Pseudo) ephedrine
• NaCl
• 
  Procedure:
  
  
  Mix the Isopropanol with the salt. This will give a lay-up solution.
  
  
  
  Pour out the top layer and discard the low layer. The lower layer will be water.
  
  
  
  Best case is the Pseudo-Ephedrine pure and already extracted from the tablets. But if not so, or there is no need crush the tablets up and add them to your isopropanol solution.
  
  
  
  Don’t add to much isopropanol, you want to achieve a sticky kind of paste. Put in the freezer for 4+ hours.
  
  
  
  While in the freezer make Anhydrous ammonia. Mix in a container ( glass!!! ) 4 parts of NaOH and 5 parts of Ammonium chloride.
  
  
  
  Set up another container wich is filled with dry ice and Acetone. The temperature must be below -33 *C. Place in that container another glass container and connect with tubing the 2 containers ( Ammonium chloride + NaOH and an empty one ). You want to make the gas that comes over when you heat it forms a liquid, and you do so by freezing the glass below -33 *C with your ice bath.
  
  
  
  Make your lithium ready. In case not extracted this is easily done by extracting lithium from AA batteries ( must say lithium ) there will be 2 metals rolled up, a shiny and not shiny metal. The not shiny is the lithium. You can test if it is lithium by adding a bit of water. In case it reacts it’s lithium. ( don’t add to much lithium + water can explode !!! ).
  
  
  
  To add your (Pseudo)-Ephedrine use the following ratio:
  
  250 ml anhydrous ammonia + 100 ml for every 28 gram ( 1 ounce ) of Pseudo. For the American faggots among us
  
  
  
  Add your ( cold !!! ) Pseudo-Ephedrine to the cold Anhydrous ammonia ( still in the ice bath ) in the correct ratio. Check the temperature. Make sure it stays below -33 *C.
  
  
  
  Wait for 7-12 minutes. Ideal there will be no temperature change. And no reaction.
  
  
  
  Break up the Lithium in very small pieces. Don’t grind it! And add a small portion lithium to your solution. The solution should turn blue! Wait till the blue disappears and repeat ( add lithium ). The lithium should be added around every 40 seconds. Until it doesn’t return back to the original color and stays blue.
  
  
  
  Stir for 30-60 minutes. Let it cool to room temperature ( 23 *C use thermometer !!! )
  
  And stir for another 60 min. You have now made Racemic (RS)-N Methylamfetamine. Now recrystallize to purify it.

 

[The Silent Chemist]

H
Has SWIY successfully done this reaction I have a couple of questions?

 

[Sascha]

Go ahead

 

[The Silent Chemist]

It is said to use freebase ephedrine/phenylpropanolamine, but it has also been said that ephedrine/phenylpropanolamine Hcl can be used aswell removing the step of freebasing the ephedrine

(not hard at all to do but it is a step in the process that could just be avoided)

Is this true ? When doing it with this method does one just follow the same protocol.

adding the lithium with the blue colour forming then dissipating and then repeating until the blue colour does not dissipate.

what ratio of ephedrine Hcl, isopropyl alcohol and anhydrous ammonia is used to accomodate for this.

apparently when using ephedrine/phenylpropanolamine hcl ammonium chloride is formed quenching the reaction?

 

[cyclic-ozone]

I would strongly advise against using the hydrochloride salt when freebasing is cheap and easy, lithium would react with the HCl salt and waste precious alkali metal.
with regards to ratios, this method was loved partially because precision is not as necessary. for example, one could use a few litres (3) of Ammonia and add to it a solution of mostly np solvent such as ether or IPA with 250g of freebase dissolved in it then commence the alkali addition.

edit F'ed up the numbers

 

[The Silent Chemist]

Here is a procedure for freebasing ephedrine, tell me what you think ?


To your ephedrine add about equal part water. Now make up a 20% NaOH solution (or 4 parts DH2O:1 part NaOH) Add Toluene or the NP solvent you want to use to water/pseudo solution about equal to water volume! Yes toluene first, it gives the pseudo somewhere to go instead of being burned by the base which can break it up and turn it into aziridines (toxic)! Add NaOH solution to water/pseudo/toluene solution till PH 13, and remember to test PH of water not toluene! Now shake the jar up very well and let settle into layers. Seperate toluene layer. Repeat this process 3 times and combine all your toluene!
You can dry the toluene/pseudo freebase with magnesium sulfate.

Ready to use in a reaction ?

 

[cyclic-ozone]

Yes, that sounds good. Best of luck I'd love to hear about the results.

 

[The Silent Chemist]

Please explain what is happening in this step Is this freebase or Hcl you are talking about ?

if this is freebase one would assume the ephedrine would dissolve in the IPA and the solution could be dried with magnesium sulfate before use. SWIM knows pseudoephedrine freebase is or could be a solid.

why is one concerned about using a small amount of IPA is this to lower the formation of byproducts “ethoxide”

 

[cyclic-ozone]

The concern of alkali alkoxides can be avoided by using an ether (sort of) and the main thing is to ensure dissolution but the drying step is absolutely necessary and oven-dried mgso4 will work because the water in solvents is incredibly harmful to the alkali metal amide formation. I think the main concern with alcohol is the exothermic reaction between alcohols and the formed amide boiling the ammonia but i am not entirely sure.

 

[The Silent Chemist]

If one is reducing phenylpropanoamine amphetamine freebase is produced. In this case after extracting the freebase from the reaction, instead of bubbling Hcl gas through the solution forming the Hcl salt would it be preferred instead to do an acid titration in IPA/actone with sulfuric acid to produce the sulfate salt

Is the sulfate salt more stable or somthing ?

 

[cyclic-ozone]

It is preferred to do the sulfuric acid titration as the sulphate salt of amphetamine is not more stable, rather, it is not hygroscopic (pulling water from the air) like the hydrochloride salt. that's why a lot of euro speed is a paste.

one could alternatively use phosphoric acid

 

[Raz]

NaOH mixed w/ NH4NO3 in a three necked round bottom flask w/ H2O added from a pressure equalizing addition funnel. Also a hose connecting to a bottle with pseudo (freebase) dissolved in coleman's camp fuel (filter through a fuel funnel to remove H2O) that has Li floating on top. Then a second hose and valve exiting bottle to vent excessive pressure.
Almost all risk of explosion should be averted, right? E.g., Ignition of Li after coming in contact with the bottom layer of NaOH & NH4NO3 while the reaction is 'rolling'. Sure it instantly goes out once the Li reaches the pressurized anhydrous NH3 atmosphere instead of air. No O2, no explosion. First hose also has three attachments; drying CaO, suckback trap, and a valve.
Clean, clean, clean. Cause it's just a single chemical as the goal. Pure dextro instead of racemic dex|levo. Sorry, started rambling in the second half.