Posted by BAD CHEMIST on February 12, 1997 at 20:32:16:
In Reply to: eph. to CAT recipe posted by Anon on February 12, 1997 at 16:17:20:
: 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...
Thank you for the great lab procedure. I think I'll reccomend it for our next lab in chem class. However, I'm a bit in the dark on something. Do you have to use pseudoephedrine? I thought that real ephedrine was a desired drug for synthesising into more powerful compounds. Also, I don't know much about CAT. Is it like Crystal Meth, or what's the deal. Thanks again.