Methcatinone synthesis by Psychokitty


              [Extraction of ephedrine/pseudoephedrine from pills]

1.) Get an amount of pills that have about 30 grams in them and grind in a
blender. Add to a large beaker or pyrex measuring cup. Extract ala Fester's
new process. I.E., add to the ground up pill powder 4 grams of Lye for every
2g of "feed stock". Mix thoroughly. Then add just ENOUGH 90% (NOT 70%) IPA
(isopropyl alcohol; rubbing alcohol) while agitating with a STAINLESS STEEL
spoon to make a paste. Mix around with the spoon for about ten to twenty
minutes. If the alcohol is absorbed during this time, add a LITTLE more just
to keep it pasty. The beaker will start to get a somewhat hot but this is no
problem. The mixture will also get a little yellowish-orange. No big deal.

2.) Mix in 1000 mL of Colman's Camper Fuel. The bluish color is no big deal.
This stuff doesn't smell half as bad as toluene so be thankful. Mix the solution
around by hand with a STAINLESS STEEL spoon for about thirty minutes swishing in
and out. From your POV, it won't look like much stuff is being extracted but
don't worry, it is. The orange powder tends to cake so this has to be done by
hand. Magnetic stirring, unlike int the video, does NOT work. The stir bar just
stands still. After thirty minutes of agitation, filter the stuff using VACUUM
filtration ONLY. You can use doubled up coffee filters as this works ideally.
Don't cut the edges off. Just work it in with your hands as the upper elevated
edges of the filter paper ensure that none of the orange powder is going to make
it past the filtration. What comes through should be a pretty bluish transparant
liquid. If you used too much IPA at the beginning, the solution will filter
through cloudy as it will have water in it. In this case you have to use
anhydrous magnesium sulfate (epsom salts) to dry the solution, so don't use too
much 90% IPA at the beginning. After all of the camper fuel has gone through,
scrap the residue back into the beaker and extract with 500 mL of camper fuel
again. Then filter and add the filtrate to the rest of the camper fuel extract.
This filtration process poses no problems in that the liquid goes through pretty
easily and without trouble.

3.) Next gas with anhydrous HCl as per usual. The crystals of "feed stock" start
to pop up soon enough and settle to the bottom. Keep gassing until you smell the
HCl or better yet, until the blue color of the camper fuel dissapears turning
transparant and colorless. Vacuum filter the solution and wash the crystals with
acetone. Then twist the filter paper into a ball at the top and squeeze out with
your hands all the remaining acetone from the filter paper crystals extract.
Allow to dry. After drying under a lamp one will notice that the smell of camper
fuel has still not disappeared. This is not good as any residual camper fuel
will react with the chromium trioxide used later on to oxidize the "feed stock",
thus reducing yields. The fuel will not completely dry even if left to do so for
eight hours! so some further cleaning needs to be done. Transfer all of the
crystals to a 500 mL flat bottomed flask. Add 300 or so mL or acetone and a
magnetic stir bar. Place on top of a magnetic stirrer-heater and connect a
reflux condeser to the top of the flask. Make sure to have either cold or room
temperature water running through it. Start the stirrer and turn on the heat to
a low setting. After thirty minutes of stirring, refluxing, and heating, the
crystals should be completely powdered and WILL be completely free of any
residual camper fuel. Filter while hot and allow to dry for about an hour.

4. Next, weigh the dried crystals. There should be anywhere from 60-75% of the
30 grams of "feed stock" expected to be in the pills. Now the "feed stock" is
ready to be oxidized into our lovely ketone product...

          [Oxidizing of Ephedrine or Pseudoephedrine to Methcatinone]

Now you have your purified "feed stock". If everything was done as stated above,
it WILL be pure and clean enough for the next oxidation step. If not, then
you're going to have a lower yield due to the using up of your oxidant by
something that is soluble in the Colman's Camper Fuel. I don't know what that
something is, but with proper clean-up, it can be removed.

For every gram of feed stock, use 10 mL of distilled water. Experience has shown
that the water from the water mills works just fine, but I wouldn't take the
chance as there is no guarantee that something in the water will not fuck-up
your reaction. Tap-water is an absolute NO-NO!

Dissolve your "feed stock" in the water. This will not occur as fast as you
might think. A little agitation or stirring is called for. Now weigh out
separately 3 grams of potassium dichromate for every 5 grams of "feed stock"
used. You'll have to figure out what amount of potassium dichromate is needed
for the reaction and then determine the amount of sulfuric acid (the OTC drain
cleaning kind is okay) needed in the reaction which is calculated as follows:
Use 3 mL of sulfuric acid to every gram of potassium dichromate used. After
measuring out the sulfuric acid, add it slowly to the "feed stock solution.
Cooling down the "feed stock" solution before this addition might increase
yields but who knows. Swirl the now formed aqueous sulfate salt of the "feed
stock" by hand. The solution will get somewhat hot but will not go above 50 deg
C (at least, it should not). Cool the mixture down to room temperature. Now you
have a solution of "feed stock" sulfate in dilute sulfuric acid. This step is
important because if one adds already formed chromic acid solution to a solution
of the hydrochloride salt of "feed stock" one gets a strange precipition that
eventually redissolves but almost always spells low yields at the end of the
synthesis. Not good. Anyway, after the solution cools, add the required
previously calculated amount of potassium dichromate and begin magnetic
stirring. This reaction is not exothermic so there is no need for thermal
control. It will take a little while for the potassium dichromate to dissolve
but eventually it will. At first, the solution is light orange and somewhat
transparant. In about an hour to two hours, however, the potassium dichromate
will have dissolved into an opaque dark-reddish-orange solution. Allow the
solution to stir undisturbed for 12 hours. The stirring can go up to 24 hours
without a significant reduction in yield, but by no means must the reaction be
halted before 8 hours. Whatever the reaction vessel used, the lid should not be
tightly closed as some gasses (harmless) sometimes form.

At the end of the reaction period the solution should look very much like when
it first became dark with just a hint of green thrown in. Usually, the color of
the solution can best be guaged by using a source of light to enhance the outer
edge of the solution, which will more clearly indicate the hue of the mixture.
If the solution has any uniform purple quality, then the original "feed stock"
was tainted (not purified enough) meaning that there might be low yields of
product. At this point, measure out a capful of IPA (isopropyl alcohol; rubbing
alcohol; 50%,70%, 91% all are okay) and add this to the solution and allow to
stir for about ten minutes. This step is paramount as it will ensure that all
the oxidant is reduced and that no chromium sludge will form at the point of
basification. The solution might get slightly hot during this period but this is
no big deal. While the mixture is stirring, measure out 7.5 grams of NaOH (Lye)
for every gram of potassium dichromate used. Dissolve this in enough distilled
water (placed in a beaker or measuring cup surrounded by an ice bath) to make a
25% solution. The beaker must FIRST be nestled in the ice bath BEFORE the
addition of the Lye or else the beaker will crack from thermal shock. After the
NaOH solution has cooled, add more ice to the bath and allow it to cool for 20
minutes more. At this point, set-up another ice-bath. Stop the stirring of the
vessel containing the solution of desired product. It should now be either a
uniform opaque marine blue color or an opaque forest green color (this varies
but both look very pretty). Place the vessel in the second ice bath and cool for
20 minutes as well. Once both the NaOH and product solutions have cooled down
for the required time, get a large 3 gallon pickle jar (empty and clean) and
transfer the contents of the product vessel into it. Pour into this solution an
equal volume of toluene which will float on top of the product aqueous solution.
Fill up the kitchen sink with water and a bag of ice. The requirement here is
only that the toluene/product solution can easily be immersed beneath the
ice-bath. Put on gloves (as the water is very cold) and quickly pour the NaOH
solution into the pickle jar. IMMEDIATELY cap and seal and begin to aggitate the
jar by hand to allow both layers of toluene and product solution to mix
vigorously and in all proportions. Do this for about one minute WHILE UNDER THE
ICE BATH and then hold under the ice bath until both layers separate. Hold the
jar steady as it will float in the ice-bath and possibly tip over spilling its
contents. Bee careful. After the layers have separated, remove the jar from the
ice bath. What should be visible is the toluene layer (possibly somewhat cloudy)
floating above a beautiful opaque forest green solution with NO CHROMIUM SLUDGE
FORMATION WHATSOEVER!!!!!. Separate the layers and wash the toluene layer with
distilled water. What should happen here is as follows: The toluene layer should
immediately grow cloudy and should separate from the water layer rather quickly
(1 to 2 minutes). If separation does not occur rapidly, then some unreacted feed
stock is still present. This is not a problem but to make separation a quicker
easier task, add a little table salt (NaCl) to salt out the toluene layer. Wash
three times. With each wash, the water layer will grow more and more clear,
until it just simply looks like plain water. The toluene layer will now be
cloudy. Dry with anhydrous magnesium salts. This will get rid of the cloudiness.
Bubble with HCl gas. The crystals of product will - unlike the crystals of "feed
stock" - form in little strings which will cling to the sides of the flask.

After gassing until there are no more crystals formed, there should be either
clean crystals clinging to the sides of the flask or alot of syrupy goo instead.
Either of these will yield the desired product. So next, decant the toluene from
the crystals and add about 500 mL of acetone. Start mixing with a stainless
steel or PVC plastic spoon, scraping the sides, etc. etc. Eventually, the
acetone will dissolve the gunk and the crystals will form. After a while there
will be either a clear or yellowish acetone solution with a goodly amount of
crystalline product floating at the bottom of the beaker. Vacuum filter these
crystals, squeeze the acetone out of the coffee filters as described earlier and
then set the filter paper along with the product out to dry. Chopping the
product under a lamp speeds up this process. Next, once the dried product is
obtained, transfer all of it to a 500 mL flat-bottomed flask and set up for
reflux and stir and heat the mixture for about 30 minutes. By the completion of
this time period, all of the pyrazine contaminant (for more information, refer
to other relevant threads of mine) should have been removed by the acetone wash.
Filter while hot, squeeze, and set to dry. Yield is about 35-50% of VERY clean
and VERY pure product. Does not burn when inhaled, and has a very bitter but
tolerable taste. Enjoy.