Author Topic: Another ephedrine->cat->meth post...  (Read 2699 times)

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ning

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Another ephedrine->cat->meth post...
« on: November 16, 2003, 03:52:00 PM »
Sorry for not putting this in the old thread, but there was no "reply" option available. This is typical Wolf-kishner stuff, but taking advantage of the nice oxidizing powers of bleach....


Double Trouble: Super easy meth from p-fed, a theoretical synthesis.

Synopsis: A simple 2-step synth that removes the need for metals, red phosphorous, and iodine. Sometimes you have to take one step backwards to get two steps forward. And to be still more felonious, you end up making two schedule-I substances simultaneously! Double Trouble!

Step 1: oxidize ephedrine/pseudoephedrine to methcathinone with bleach. (NaOCl)
Step 2: reduce the methcathinone with hydrazine, Wolf-Kishner/Huang-Minlon style.

Two sets of papers make this route seem very feasible. First, the slew of papers on the use of TCCA and NaOCl to oxidize all sorts of primary and secondary alcohols to aldehydes and ketones in 80-90% yield. Some use phase-transfer catalysts, others do not. Acetic acid & NaOCl has been done, as has TCCA and acetone. Perhaps NaOCl and acetone? Also, if PTC is necessary, it just means adding some fabric softener or dishwasher detergent. Nothing too difficult. Oxidation is simple, fast, and efficient at room temperature, for 10 minutes to an hour, with 30 minutes being normal.  Secondly, the Wolf-Kishner reduction is a classic reaction that is well documented. A simple ketone such as methcathinone should be no great challenge. It may be possible to use just water as the solvent and perform the reduction at reflux, otherwise ethylene glycol is a high-boiling solvent commonly used for WK reductions. Hydrazine is easily synthesized from bleach and ammonia. See Organic Syntheses "Hydrazine Sulfate".

It may be possible to perform the above synth in one pot, by adding p-fed, oxidizing in bleach, then adding more bleach and an excess of ammonia to form hydrazine, adding hydroxide to decompose the hydrazone, and heating up the pot to reduction temperature, letting all the low-boiling things come off along the way. If this does not work, the hydrazine can be removed as the sulfate and a standard two-step synthesis mode employed.

Total bill of materials should look something like this:
Acetone
Bleach
Ammonia
Toluene/xylene
Sulfuric acid

Pseudoephedrine pills and the necessary extraction solvents (gakks keep changing, after all)

The pathway is something like this:
 


   Extract pseudoephedrine                 Make Hydrazine
    From pills                            Bleach + Ammonia.
   Toluene, ammonia, etc.                Extract as sulfate w/ H2SO4
                  |                           |
                  |                           |
        Oxidize p-fed to cat              Perform Wolf-Kischner reduction
        use bleach & acetone ----------->  use hydrazine & cat
                                              |
                                              |
                                          Extract and clean up your meth
                                            use toluene & water.
                                          Precipitate it as HCl crystals.



Except for the pseudoephedrine, this path is basically uncontrollable. Until every household chemical is watched or gakked up, this path should work and be safe (if it works at all). For those who only want to make a small supply of their own stuff from a box or two of p-fed pills, this could be the safest and easiest way.Also, though the hydrazine is poisonous, the nasty waste generated is much less than RP/I or (ugh) aluminum amalgam. Have to find out what common material can destroy the excess hydrazine safely, though.
Yields to expect: Oh, say, between 50% and 70%, based on typical yields of the two individual steps.


Rhodium

  • Guest
protecting group needed
« Reply #1 on: November 17, 2003, 02:32:00 AM »
If you read the old threads on the topic, I have described why this will not work without a protecting group on the nitrogen atom.