METHCATHINONE via
K2Cr2O7
By XplosiveKemistry
Cleaning Ephedrine
Several methods exist for the
cleaning of pseudo-ephedrine, for thoroughness I will note "The Cure", written
by the great Ozbee himself, which is a very detailed and preferred way to
extract the pseudo-ephedrine from pills.
I recommend highly using a cleaner extraction method than the one I present
here, but this will work in a pinch!
Start off by using any number of pills (use at least enough to make it worth
while, but I've used as little as 2 gm). Make sure the pills don't contain
acetaminophen (Tylenol), povidone, or guafinesin, as these will surely spoil the
synthesis! These were cleaned in a very fast manner, again, may not be advised,
to obtain optimum yields.
I started with 1440 pills of pseudo-ephedrine and placed in a wire mesh and
put in an equal 'volume' of crushed ice. The cold, abrasive nature of the ice
will remove the red coating and minimize the water erosion of pseudo-ephedrine
from the pills. It is also acceptable to slowly trickle distilled water over the
pill bunch to further remove the red, but take caution: excessive d-H2O will
drop yields due to minimal loss of pseudo-ephedrine, so take it easy Once pills
are cleaned in this manner, place in a 500 ml flask and add 200 ml of d-H2O.
Place in microwave and let 'cook' ONLY UNTIL CONTENTS ARE HOT TO TOUCH, BUT NOT
BOILING! This is one of only three critical points, so take care to do this
properly. When this is finished, let the filler material settle and prepare the
vacuum filtration. Liquid will still have a pink tint to it if cleaned as I did,
but this is no big deal. Either decant this liquid slowly as not to disturb the
gakk settled in the bottom, or can pour it all in the filter and clog it all to
hell.
This WILL work, however, but you will probably spend more time scraping
residue from the filter and waiting for it to finish than anything else, so my
suggestion would be to decant, only a small amount of residue will fall into the
filter and it will not need to be scraped for reuse unless using a smaller
amount of pseudo-ephedrine. Repeat this procedure 3-4 times, or until the filler
residue is no longer bitter. In any event, make sure the glassware will sustain
the volume of liquid, as you will have double this amount of volume at the free
base/extraction stage later on. Place this in a 1000-ml flask and put on a stir
plate; drop in small stir bar and let stir.
Oxidation
Dissolve the ephedrine in water using
this formula
under 1 oz -- use 30ml per 1gm of E
over 1 oz -- 250mls
(initially) + 25mls per 1 gm of E used over 28 gms
Measure out 0.5 gm
of K2Cr2O7 (potassium dichromate) to every 1.0 gm of pseudo-ephedrine. Add
dichromate while stirring the pseudo-ephedrine and let settle as much as you can
while it’s stirring. Liquid will turn a bright orange color as the dichromate is
added.
*(NOTE: NO coldness was needed in this process so far, but get ready,
it’s coming.)
After making sure all of the dichromate particulate has indeed
dissolved, slowly add sulfuric acid (98%) at 3 ml per 1 gm of pseudo-ephedrine.
This brings us to the second critical point: Add this H2SO4 SLOWLY, as adding
too fast will concentrate acid and it destroys pseudo-ephedrine, so go slowly or
lose product! The orange solution will now start to get a dark color as the
reaction takes place. On larger batches, if foam up starts, simply remove flask
from stir plate and let settle, or help settle it with a glass rod or a
STAINLESS STEEL butter knife. All you are trying to do here is settle the foam
down and not panic. Easy problem, easy solution! Upon completion of adding acid,
(liquid will be slightly warm, almost hot during this entire addition of acid
stage, so it's OK) let this solution do it’s thing for 45-60 min. You will not
want to go less than 45 minutes. Because I really don't think it gives the
reaction time to take place, although, I've never been patient enough to go over
60 minutes.
This would be a really good time to grab a smoke/ drink/ whatever.
While
the oxidation reduction reaction is stirring for this hour or so, you can do
some other things to prepare the rest of the process,
Preparation of the lye solution
Red Devil lye
was used here, 100 gm NaOH was slow dissolved in 400 ml of d-H2O. **DO THIS
SLOWLY, ADDING THE LYE IN 25 gm INCREMENTS, and ALLOWING IT TO DISSOLVE AND COOL
TO THE TOUCH BEFORE ADDING MORE. If you cannot do this slowly, you will most
probably burst the flask due to either thermal shock or superheating it to the
point that you can no longer hold onto it, thus dropping it on the awaiting feet
below, so you may want to consider placing the water in an ice bath BEFORE you
add the lye so as to avoid the whole thermal shock thing. Remember that you have
a whole hour to do this, so take your time.
Slow down reaction use ice
After 60 minutes the
oxidation reaction time is up. Remove the stir bar, and place the whole flask
into an ice bath. This is our third and last critical point: Notice this is the
first time ice has been used on the reaction solution. Let the reaction mixture
chill for 30 minutes. or so to stop the oxidization and to insure that no
thermal threats will occur, as you do not want this oxidizer/acid solution
pouring from a cracked flask and on to anything that may be attached to you.
Freebase
Add lye Chromate Turns Green
Upon the completion
of the 30-minute chill time, slowly pour the d-H2O/ lye mix (which should now be
clear and slightly warm--maybe more than slightly, depending on how recently you
made it) slowly to the oxidizer mix. You should at this time notice wisps of
smoke coming from the mix. Relax, it's normal. You are looking for the mix to
turn pale greenish. If it doesn't turn after all the aqueous lye solution is
added, simply add more lye, although it is not necessary to dissolve it in d-H2O
this time, simply pour it in slowly (think: teaspoon at a time) until it does
turn green. You will start to smell the characteristic ‘pistachio’ smell, but be
careful if the reaction goes back to a dark color, you will have burned the
product. I don't know why this is, but YIELDS WILL SUFFER. Pour off a little of
the base and test the pH, it should be at pH-12.5+, if not, add more lye at VERY
SMALL increments--remember, you don't want to over gasify. I've had luck pulling
a base of pH-11 or so, but the yield wasn't great.
The Goods
At this point, you will be enticed by
the great smell of the pistachio, but never fear this is about to end! As soon
as you get the base pH right, you may then remove this from the ice. Pour into
the base about 300 ml of a non-polar of choice: Toluene, works best but
availability may be limited Xylene, dries a little slower than toluene, but
works the same Coleman’s camp fuel, always an option but any source of Naphtha
will work in a pinch situation *Naphtha seems to leave an oily residue in the
free base that isn't easily dried out when the CAT becomes an HCl-salt, so use
it if it's the only thing you can find. Agitate this Toluene-base mix and let
settle. The Toluene will rise to the top with the CAT free base in it. It will
be an off clear to yellowish pale color. Decant this Toluene layer into a
separatory funnel. You can do this twice cleanly but the third extraction will
most likely yield nothing worth the time and effort. Do not allow any of the
sludge to enter Sep funnel, pour only the Toluene into it, as this contains the
product.
Make CAT water soluble
Add diluted HCl/d-H2O
mixture to this...I used a 10% mixture and adjusted the pH as needed. My
solution was 100 ml of 32% muriatic acid in 1000 ml of d-H2O that was prepared
beforehand. ! You will see the water/acid/CAT fall to the bottom after you shake
a few times, let this settle shortly You will be looking for a pH below 7.0 Then
drain off water/acid/CAT into a beaker of appropriate size. Place on an electric
stove with low to medium heat, or if you have one, place on a heating element
not to exceed 150 F in either case. Let this heat until liquid turns a pale
amber color or has evaporated 1/2 of the fluid away.
Microcrystals with acetone
Addition of some
Acetone will form micro-crystals. These will be barely visible sized crystals
and there won't be many, keep boiling and adding a little acetone looking for
the crystals. We ain't done yet! When crystals begin to form Place in flask and
seal with correct size stopper. Place this in the freezer for about 15-30
minutes. checking periodically to insure coldness, but not to the point of
freezing!!! When chilled sufficiently, flood flask with ices cold Acetone (when
the Acetone fills to the bottom part of the neck on the flask, this will be good
enough). Shake vigorously for a few seconds and watch the crystals form and
settle in the flask. This is the CAT in a soon to be consumable form. Let all
crystals settle and strain through 2 coffee filter.
Removing the NaCl
Consistency of dried, uncut
CAT will be slightly rocky, but otherwise like powdered sugar. Once the CAT has
been produced and has been semi -dried, we need to remove nasty NaCl and other
salts that appear in the final product. While still in the filter add some dry
alcohol such as Methyl alcohol (Methanol) or Denatured alcohol. Dissolve as much
of the dry CAT powder into denatured alcohol as is possible. (The (salt) NaCl
will not dissolve) The filter traps unwanted salt Collect the liquid
\Cat/Alcohol in and a clean flask or bowl. Bring the CAT/alcohol to a slow, soft
boil. DO NOT LET THIS MIXTURE OVERHEAT! Keep a constant surveillance on this at
all times and NEVER do this over an open flame or other source of ignition, use
a warmer plate or a hot plate with a temp regulator.
Final re-crystallizing
As soon as some crystals
form, seal the container up tightly and place in the freezer for approx. 8-12hrs
for re crystallization. Pure CAT will slowly form; the crystals will be tight
and clean. Filter the crystals to remove the alcohol. While in the filter
lightly rinse away all alcohol and residue from the crystals with a splash of
cold dry acetone. Let air dry, and enjoy!
Comments
Yield on this synthesis should be at
80% or higher, depending on how clean the pseudo-ephedrine is. One needs to
exercise extreme caution that at no time a flame is introduced around Toluene,
Denatured Alcohol, or Acetone, and the recommendation of some light rubber
gloves would make acid handling safe. This synthesis was reconstructed for
simplicity and consistency, as well as my own personal experience of trial by
error. All elements here key off the use of pseudo-ephedrine in grams, NOT
MILLIGRAMS, so adjust weight accordingly! None of these chemicals are on the
highly dreaded watch list and most can be had right from hardware stores and
Wal-Mart.
XplosiveKemistry
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