Post from Hive 2003:
NEEDED FOR PREPARATION:
Collander w/ reletively small holes
Pseudephedrine tablets, 100 of 30mg each.
Acetone or Ethyl Ether.
Potassium Permaganate crystals, of reasonably pure origin
[no lead, other toxic metals allowed. Sodium, Chloride, other
pharmalogically 'safe' contaminents are OK]
Purified water [TAP WATER WILL *NOT* FUNCTION ADEQUATELY IN MOST CASES]
Refridgerator chilled to just over 0c.
Turkey Baster or other method of measuring water in mililiter quantities.
An area heated or chilled to "room temperature" (ROUGHLY 25c or 75f)
Acetone or Ethyl-ether for the washing [not needed for smokable form]
MEASURING OUT & PREPARING THE KMnO4 FOR REACTION:
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).
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.
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.
EXTRACTING AND PREPARING THE PSEUDEPHEDRINE HCl FOR REACTION:
****synthesis I recieved originally read:
| Purified water (roughly 250mL) is added over the cleaned pseudephedrine
| tablets and heated until hot to the touch [outside of jar] in a microwave
| at low power [eqiv. about 150watts]. This takes about a minute.
| Solution is stirred once every minute, until tablets have completely
| fragmented. Solution is allowed to settle, and poured off thru a coffee
| filter. Powder remaining in bottom is again covered with 250mL water and
| heated until hot, stired, allowed to settle, then poured thru same
| coffee filter. Any powder in coffee filter is replaced with "filler
| material" from the tablets, and covered with yet another 250mL of water,
| heated until 'hot' and once again, for a final time, extracted thru a
| different coffee filter (the old one crumpled up).
************ but later I "translated" to this for public convienence:
* Place the just washed and probably slightly red pseudephedrine tablets in
* a jar, and pour 250mL of water over them. Now heat this in a microwave at
* low power until it gets "hot" but not to 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 250mL 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 250mL and heat until "hot". This time pour thru the filter,
* and your done.
The pseudephedrine solution, about 700mL or so (okay, so some water gets
away, or I measured wrong, or the 'salty' nature of PfedHCl caused the H2O
to contract, or... the list goes on) is placed in the fridge to chill, next
to the KMnO4.
NOW THE FUN BEGINS (THE REACTION):
After a few hours, the two cold solutions are mixed together,
stirred, and replaced in the fridge overnight (12 hours).
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, stirred, and this is allowed to come to room temp. on its
own over two hours.
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.
This final 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'. In any case, the solution was made slightly acidic with conc.
HCl and many, many measurements of pH.
MAKIGN GLITTERING WHITE CRYSTALS:
If not yet, during this part of the proceedure you will definitly smell
the methcathinone. smells pleasent.
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 (maybe 5 to 6?). This will ensure that Methcathinone HCl is produced, and
not the freebase, which can decompose easily. While the original author of
this synethesis used 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...
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
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 will 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 with a better solvent later (see next paragraph).
Washing the crystals with ethyl-ether is definitly the way to go, as it
avoids loss and dries far quicker than acetone. Ethyl Ether, when used to
dry the methcathinone of its oily residue, then pooled and evaporated
elsewhere contained no readily discernable crystaline material - a strong
testament to the insoluability of HCl salts in ethyl ether.