Posted by Anon on February 12, 1997 at 16:17:20:
In Reply to: Ephedrine posted by Mrk -Wpg Mb on February 12, 1997 at 15:30:57:
Synthesis Ingredients
Collander w/ reletively small holes
Shaved Ice
Pseudephedrine tablets, 100 of 30mg each.
Reasonably pure KMnO4 (Potassium Permaganate). Avoid lead and other toxins.
Distilled water. TAP WATER WILL FAIL!!! Purified water usually works.
Refridgerator chilled to just over 0c (most are).
Small turkey Baster or other method of measuring water in mililiter quantities.
An area heated or chilled to "room temperature" (ROUGHLY 25c or 75f)
Isopropanol for quenching KMnO4... 70% to 100% is OK if its clear.
Ethanol optional for speeding drying process.
Acetone for the washing of crystals.
Most kitchens do NOT come equipped with a scale capable of measureing individual grams, let alone miligrams. And in many
states, possession of such a finely tuned instrument, while not a crime, certainly is admissable as one of many items of evidence
to be used in a criminal investigation. Definitly something to be avoided. Keep all the ingredients and all the labware in its
"everday-use" place, and there's no evidence to support the existance of a cat lab. And no need to manufacture the stuff in the
high desert regions either, since weird scents are for the most part avoided.
Extracting Pseudephedrine HCl
(kudo's to POPeye for his document "Getting the Red out") 100 of the 30mg generic pseudephedrine tablets were placed into
a collander containing about the same "volume" of crushed ice. They were swirled around in this collander over a sink (with
running water to wash the color down the drain) until all the ice had melted and washed thru. The tablets were then rinsed once
with distilled water, and removed to a glass jar for extracting.
NOTE: The running water kept the drain clean, but wasn't ever in contact with the tablets themselves. This
confused a number of people. Obviously, its not necessary for this... just convienent I guess. Do not wash the
tablets UNDER WATER with crushed ice. Rather, place them in the colander with crushed ice, thats it, and stir
them around,.. The very cold ice does a minimum of disolving WHILE its abrasion removes the coloring.
Place the just washed and probably slightly red pseudephedrine tablets in a jar, and pour 150mL of water over them. Now
heat this in a microwave at low power until it gets "hot" but not boiling. Stir the crap until the tablets fall all to pieces, then let
the powdery FILLER material settle, leaving pseudephedrine in solution all by its lonesome, or at least mostly by its lonesome.
Slowly pour this THRU coffee filter into another jar.
When this is done, scrape/shake/get any powder caught in the filler and stick it in the FIRST jar, the one that might have some
sludge at the bottom still. Now add another 150mL of water, heat until "hot", stir, then let settle. Pour this thru the coffee filter.
Get the powder stuck in the filter (again) back with the sludge and add still another 150mL and heat until "hot". This time pour
thru the filter, and your done.
It is worth noting that the filler material clogs the filters and will dramatically increase time for filteration to take place, like from
30 seconds to 30 minutes. The enlightened will at once realize that the easiest way to avoid this is to decant, or pour slowly so
as not to disturb the sludge at the bottom, the solution thru the filter first, waiting until its really necessary to dump the sludge
onto the filter. Also, avoid dumping "dry" sludge onto the filter, the only sludge that ought to be on the filter is that which
became dispersed in the water while pouring. In an ideal world, everyones kitchen would have a centrifuge (and a miligram
scale too!) and this wouldnt be a problem, but then again in an ideal world we would be able to buy our drugs over the
counter, and not have to make them. Suffice to say this isnt an ideal world.
Measuring and preparing the KMnO4 solution
KMnO4 is saturated at 25c in water - 100ml of solution holds 7.43g This time I will be using just under 3g of pseudephedrine
(if extract was perfect would be exactly 3g pseudephedrine). Keep in mind that when preparing the saturated solution you
need room temperature and time - you need to let the crystals settle!!! Excess (undisolved) KMnO4 will stay "swirled in" the
solution. Let it settle for a while at room temp, _then_ measure the 15mL or so... Failure to do this will result in a failed
synthesis. If you are too impatient to do this, then you should purchase a miligram-quantity scale.
In acid conditions, 1 mole of KMnO4 will oxidize 5 hydrogens. In basic conditions, 1 mole of KMnO4 will oxidize 3
hydrogens. We won't be specifically using either, because KMnO4 also works nicely under neutral conditions.
It can be reasonably anticipated that the Pseudephedrine HCl will posess somewhat of an acidic character, so we will 'assume'
acidic conditions, which also will allow us to avoid using TOO MUCH KMnO4... small amounts of pseudephedrine will go
unnoticed in the final product, but gooey messes will not, for obvious reasons.
The Pseudephedrine/KMnO4 ratio should be 2.5Mole to 1Mole, according to previous calculations. 3g pseudephedrine is
18.15mMole, therefore 7.26mMole of KMnO4, or 1.148g will be needed for the reaction. This means that 15.45mL of
concentrated solution at room temperature will be needed. Obviously us kitchen chemists can't be that precise, so aim a little
high, as previous margins were set about 10% low... use AT LEAST 15.45mL prepared at AT LEAST 25c.
Preparing for the Cold Reaction
This 15.5 or so mL of solution is then diluted with 250mL H2O, and is started chilling in a refridgerator, with just over 0c the
goal. Place the pseudephedrine solution in the fridge to chill, next to the KMnO4 solution. Label the jar so that in the event you
are raided during the proceedure, the feds will know which evidence is which and have a handwriting sample to implicate you
in the manufacturing process. Leave the jars to chill (at least 4 hours, maybe more. Check temperature if your unsure - it ought
to be just slightly above 0c or 32f)
And for the next few hours, nothing happens. This is a good time to stop for lunch, if your into eating.
It should be noted at this point that much feedback has been recieved from "failed" synthesis caused entirely by
not letting the mixture chill long enough. If your impatient, place it in the freezer until ice begins to form then allow
it to warm just enough to melt before mixing remember, the ONLY reason this works at all is because the dilution
and temperature are such that the permaganate oxidizes the alcohol to a ketone and GETS USED UP before it can
do anything damage. Make the solution much more concentrated or much warmer, and these guarantees may not
work.
The Reaction (the boring part??)
After chilling, the two cold solutions are mixed together, stirred, and replaced in the fridge overnight (8-12 hours). This is a
good time to stop and have dinner, pork your significant other, and then get some sleep.
In the morning, instead of a PURPLE color in the jar, there is a mostly clear layer, and a brownish gunk on the bottom, which
agitates easily. Because its safer to err on the side of caution, 100mL of 70% isopropyl alcohol is added and stirred.
If a purple color remains, odds are that an EXCESS of KMnO4 was used and the synthesis will fail, or that not enough time
was allowed for the reaction to take place. Do not allow more than 12 hours in any case, instead give the KMnO4 something
else to chew on [the isopropyl alcohol]. This is the sole reason for the addition of isopropanol. Ethanol or methanol were not
used because they tend to oxidize further to substances not so easily seperated from the product. Any acetone made from the
isopropanol will evaporate easily.
Let the mixture sit for roughtly 2 hours on a shelf, and at the end of this period it should be around room temperature. Time to
room temp will vary with dimentions and thickness of the container, of course.
This mixture is filtered thru two coffee filters stacked on top of each other with the intention of catching all the little maganeese
particles that have precipitated. In an ideal world, you can do this on the first try and get a perfectly clear liquid on the bottom.
In a less than ideal world, it was necessary to again RECOOL SLIGHTLY the filtered mix, and filter this thru another pair of
coffee filters. My hunch is that the slight cooling in the fridge, and/or the extra time allowed the rest of the maganeese to 'clump'
together into pieces too big to escape unfiltered.
Many have found two, three, or even four refiltrations to be necessary apparently the choice in coffee filter places
a dramatic role. The truly patient chemist could use a PAPER filter, provided it is free of anything that would end
up in the mixture, such as coloring. The well equiped chemist would use a paper filter and a vaccuum suction device
that would pull the stuff thru the filter paper, but hopefully not rip it. Perhaps such a device could be built in a
manner similar to a bomb, with the place where the mouth goes used to hold the filter, and the place where the bowl
goes hooked up to some kind of suction (an aspirator, mini vaccuum, I dunno). The contents of the bong would be
the desired part...
| |
| |// A bong. This one is underfilled, of course, because allowing
| '/ it to fill completely would be potentially waste product on
|~~| the vaccuum rig.
_|__|_
The bong idea is totally untried, but it seems like a sound idea.
This final, filtered solution was found to be basic with a pool test kit, no suprise if you figure that the HCl part of the Pfed was
used up in the oxidation as 'acid'. Results will vary on the final pH. If its already acidic, you dont need to add any more acid
(heheh).
Most have found a pool test kit woefully inadequate, and have suggested using pH paper. I almost wonder if the
amateur pH meter made from boiling red cabbages wouldnt be better than a pool test kit, as it is also wide range.
See Mr. Wizard or any high school chemistry book for details.
Purification - making glittering white crystals
If not yet, during this part of the proceedure you will definitly smell the methcathinone. It has a stronger odor than
methamphetamine, BUT the odor of methcathinone is _pleasant_, even to those who have not experienced the drug (some
people LEARN to like certain smells, but cat just smells plain good.)
The smell has been most closely likened to pistacio ice cream, of all things. Will wonders never cease...
Considering the fact that there's either isopropanol or acetone in the above mixture, its probably not a wise idea to just load
your rig straight from it and shoot. And considering you might want to give some of your creation away, it'd sure be nice to
have a transportable form.
NOTE: A *very small* amount of conc. HCl is required. Add it one drop at a time with stiring.
Now to make sure the stuff is indeed the HCl form...
Add HCl with stiring to adjust the pH to slightly acidic, i.e. just under 7 (like 5 - 6.5). This will ensure that Methcathinone HCl
is produced, and not the freebase, which can decompose easily. While the original FAQ suggesting using a pool test kit to
measure the change in pH across a very narrow range, many people haven't got this to work, and instead a less sensitive agent
[pH paper?] is reccomended. Perhaps even the classic "red cabbage" pH tester will work... see any kids chemistry book for
more details on this plant-based pH test... In any case, if its concentrated HCl, add it ONE DROP AT A TIME with stiring
and checking of the pH. If you add too much HCl, the crystals wont seem to dry out properly. Fear not, place them in a
freezer or some such, then take them out let them thaw & dry more, they will eventually freeze *after* the excess HCl moves
into the atmosphere.
Pour the stuff into a glass (PYREX!) brownie dish. Place on a stove and heat gently from below _while_ blowing lightly with a
hair dryer (avoid splashing - it wastes drugs and leaves residue.) Eventually there will start to be a really really thick gooey
mess. Adding methanol or ethanol to this thins it while speeding the drying process - a definite plus. In my case, ethanol was
used, although methanol may be preferable. Doing this is probably a must to dry the crystals at a reasonable temperature in a
reasonable amount of time, unless you happen to have a vaccuum pump lying around....
While it would seem that adding liquid would increase drying time, this is not the case because the alcohol helps
remove water from the crystals - almost dry crystals can be heated very hot and still not dry. For best results do
not add the extra alcohol until the drying stuff is kinda thick, or the first crystals have started to form.
Be careful not to overheat the crystals. If they MELT, you've almost definitly screwed up.... :)
Washing the crystals with acetone _is_ a possibility but can dramatically reduce yields, as Methcathinone HCl is apparently
pretty soluable in the stuff. Just save the acetone and let it dry all alone, somewhere, for a product that is smokable but too oily
to chop & sniff... Methcathinone is easily recovered from an 'acetone-wash' by slow evaporation, and such recovered
globs/hunks/crystals/slime/ooze/whatever you get should be saved and washed again, to recover any lost crystals.
Strangely, certain solvents will affect the potency of the end product. Disolution of the base in methanol will result in
racemization! If you are especially (dis/) pleased with the results of a particular batch and can't figure out why, think back to
what solvents were used in drying and/or washing.
Testing your CAT
BURN: A burn-test of acetone-washed methcathinone left almost NO residue. The methcathinone HCl was heated over
methane flame in a spoon. It first melted, then began boiling, and finally literally BURST INTO FLAMES and was gone except
for a spot where the spoon was possibly corroded.
A burn-test of the oily methcathinone from the acetone wash which evaporated (and would have been lost had I not kept the
byproduct of the acetone wash) performed the same way! Its oily nature prevented clean chopping, but upon washing with
ethyl-ether good product was formed from this oily cat.
A burn-test of ether cleaned acetone-wash extract left nothing behind but a slight discoloring of the shiny part of the spoon,
probably due again to reaction with the HCl or reaction with air catalysed by the salt nature of the crystals (?)
TASTE: Bitter. No evidence of numbing of the tounge or sinuses was evidenced. Snorting the product produced intense
burning feelings in the nostrils, stronger than saline solution or (laughably, I did this once to prove a point) sugar (which doesnt
feel at all!), about as much sting as with methamphetamine, and no where near as much sting as was once obtained from
snorting diphenhydramine concentrated from benedryl (a very stupid experiment in nasal congestion...)
SMELL: Typical of a ketone - sweet. Once report says it smells like "pistaccio ice cream" when wet. The dry crystals dont
smell all that much, but it doesnt take a genius to realize that once they get dogs trained for this stuff detection will be simple.
The melting point of the HCl form is 182-184c according to listing below. The CAT produced in this proceedure melted
somewhere withing plus or minus ten degrees of this temperature, the thermometer wasnt all to great...