November 21, 2014, 05:25:53 pm

Author Topic: Methcathinone - cold reaction w/KMnO4  (Read 6402 times)

0 Members and 1 Guest are viewing this topic.

Offline DOM

  • Fledgling Contributor
  • Posts: 43
Methcathinone - cold reaction w/KMnO4
« on: November 18, 2006, 04:25:54 pm »
I overheard someone discussing this reaction with a friend and they couldn't seem to agree on many points. The most critical of which was did this cold synthisis using potassium Permaganate really produce "cat" or did it convert into benzaldehyde? Also since the amount of KMnO4 is critical to the amount of efed, at which tempertaure should you extract it from your7.43gr per 100 ml solution since the temperature dictates what concentration level the KMnO4 will be at, room temp or cold temp? For 3 gr of efed 1.45ml of the saturation liquid of KMnO4 is needed. Or can you just use 1.146gr of lab grade pot. perm. and toss that in to your cold efed water solution and shake the s**t out of it and put it in the refer till it's ready. Those guys just couldn't agree on anything. Maybe with some help I can join in on the discussion and set them straight on at least a few points. I've looked around at some of the more prominant sites and saw a lot of what they were talking about so I'm looking for alternatives to those places or maybe some other knowledgeable places or people. (Does that last sentence sound right?) I am getting tired
uncle bob

pylkko

  • Guest
Re: Methcathinone - cold reaction w/KMnO4
« Reply #1 on: November 18, 2006, 06:53:16 pm »
First, are you aware that it is easier to make methamphetamine from ephedrine in good yields? Your post is not clear, I asume you are using racemic ephedrine and not pseudo, since from what I've heard it is more difficult with pseudoephedrine. What exactly are you asking wiht "at what tempereture"?

THe only thing relevent AFAIK is how long the reaction takes place, i.e that you don't overoxidize it, decompose it. It smells good as is greenich brownish colored when you want to end the reaction.

You can use other metods also  for cath, you can use the frozen H2O2, method, you can use the US2802865 patent (preparation of methcathinone by oxidizing ephedrine with sodium dichromate in H2SO4/water) etc.

pylkko

  • Guest
Re: Methcathinone - cold reaction w/KMnO4
« Reply #2 on: November 18, 2006, 06:58:16 pm »
Post from Hive 2003:


NEEDED FOR PREPARATION:
Collander w/ reletively small holes
Shaved Ice
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
lying around....

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.

Offline DOM

  • Fledgling Contributor
  • Posts: 43
Re: Methcathinone - cold reaction w/KMnO4
« Reply #3 on: November 19, 2006, 01:06:21 am »
Thank you very much, You managed to not answer anything I asked.  I stated that I checked all the major sources, hence your posting of the synthisis from Erowid doesn't help. Let me rephrase a few items for you since I am wide awake today as opposed to falling asleep after a rough day at work yesterday. Maybe I was a little vague but last time I just came right out and said what I wanted, how I wanted, my post got deleated and I got a warning so I'm trying to stay within the limits here. After all I am only a "minimal contributer" and I don't have a lot of time logged on this site,but I do have a life outside of my computer. Anyway, someone said that this synthisis produces primarily benzaldehyde and a small amout of cat. I find discussion on both, which is it? Second, the density of the KMnO4 solution changes with the tempertature (cold or warm), does that have any bering on how much solution you use from your 100 ml mixture? And if you can make methamphetamine simpler and with just as easy to obtain chems, I'd like to hear it. Not anhydrous ammonia is it? 
uncle bob

pylkko

  • Guest
Re: Methcathinone - cold reaction w/KMnO4
« Reply #4 on: November 20, 2006, 04:15:21 am »
You are very welcome! I think that you shouldn't feel such low self esteem, afterall the little title things are probably not taken seriously by anyone here.

Ketones are generally difficult to oxidize, that is as compared to aldehydes. Thus you need to use strong oxidation agents, which sometimes can distruct the molecules, by breaking carbon-carbon bonds. Thus in the reaction oxidation will lead to both methcathinone and on the other hand through destruction to benzaldehyde. It is not an either or question. The yield of your reaction will correlate with the method used and how much (over)oxidation takes place. In general this reaction is hard to do with potassium permagnate and it is easier to protect the product in reaaction that occur in acidic conditions using other oxidizers such as dichromates or sodium hypochlorite.

You should calculate your amount of oxidant in moles and forget about the density.

AS for meth? Hypophosphorous acid, by purification, distilling sodium borohydride?

Offline DrYRHead

  • Uberator
  • Ultimate Contributor
  • Posts: 9529
  • Sally as the cave
    • http://www.elfstarstudios.com/rabbit-hole.html
Re: Methcathinone - cold reaction w/KMnO4
« Reply #5 on: November 20, 2006, 11:18:55 am »
There has not been too much talk about cat of late. Whatever the case, this thread could really be transferred to the Den.
DrYRHead

Welcome to the rabbit hole.

Offline faksuo

  • He is Risen! Our Forum Messiah!
  • Forum Spammer
  • Posts: 747
Re: Methcathinone - cold reaction w/KMnO4
« Reply #6 on: November 20, 2006, 12:51:45 pm »
Quote
THe only thing relevent AFAIK is how long the reaction takes place, i.e that you don't overoxidize it, decompose it. It smells good as is greenich brownish colored when you want to end the reaction.

Think you are getting your reactions mixed here or something, u.  He's talking about the KMnO4 rxn which should go from dark purple/black to clear with brown MnO2 precipitating out upon completion of the rxn.  The potassium dichromate cat synth goes from red-orange to green-brown to green after basification.

To answer DOM's questions: the whole point of measuring the solution of KMnO4 is for people who don't have a scale.  The idea is to completely saturate however much H2O with KMnO4 at room temp, so that when you measure out 15.5 mL, hopefully it is equal to 1.43 grams KMnO4 in solution.  If you have a scale just weight it out.  The theory behind the cold temps is that it will reduce the oxidative power of KMnO4 so that it doesn't turn the majority of your product into benzaldehyde.  This is why the instructions call for placing the reaction mixture in the fridge.  Some benzaldehyde is produced during the reaction but some cat is also produced.  In what quantities, I do not know.  SWIM did this KMnO4 rxn a few years back.  He did get some product, but did not have a scale to measure it out.  If you do the reaction and end up with some powder that you can snort, it is probably cat, as benzaldehyde is a colorless liquid at room temp, and not easily snorted.
still in machine-like stride

Offline DOM

  • Fledgling Contributor
  • Posts: 43
Re: Methcathinone - cold reaction w/KMnO4
« Reply #7 on: November 20, 2006, 01:32:32 pm »
Mahal, you are a credit to the cause. Most definately much help. And I thought that maybe I wasn't asking the right questions, but at least you understand me. But is that good? or bad for both of us? just kidding. Thanks
uncle bob

Offline DrYRHead

  • Uberator
  • Ultimate Contributor
  • Posts: 9529
  • Sally as the cave
    • http://www.elfstarstudios.com/rabbit-hole.html
Re: Methcathinone - cold reaction w/KMnO4
« Reply #8 on: November 22, 2006, 04:02:53 pm »
First, are you aware that it is easier to make methamphetamine from ephedrine in good yields? Your post is not clear, I asume you are using racemic ephedrine and not pseudo, since from what I've heard it is more difficult with pseudoephedrine. What exactly are you asking wiht "at what tempereture"?

THe only thing relevent AFAIK is how long the reaction takes place, i.e that you don't overoxidize it, decompose it. It smells good as is greenich brownish colored when you want to end the reaction.

You can use other metods also  for cath, you can use the frozen H2O2, method, you can use the US2802865 patent (preparation of methcathinone by oxidizing ephedrine with sodium dichromate in H2SO4/water) etc.

Either l-ephedrine or d-pseudo' have been used. Both oxidize into the racemic-methcathinone via either the Jone's(dichromate+H2SO4+H2O) reaction or the cold reaction(KMnO4+H2O)  were used upon either precursor. As cat from street sources that has been analyzed is all of the racemic isomer.

BTW, one has heard that the H2O2 method does not work, at all.
DrYRHead

Welcome to the rabbit hole.

pylkko

  • Guest
Re: Methcathinone - cold reaction w/KMnO4
« Reply #9 on: November 22, 2006, 10:53:43 pm »
Yes, you are correct I mixed the colors up in my head, I just did a quantative (color) titration of H2O2 today using potassium permagnate and yes, the color went from that dark purple to clear upon hitting the solution untill it had reacted all the peroxide. However, regardless of the colors, you should just calculate the amount needed in moles from the electron balanced reaction and aim for something in that range, and taking further advantage then of "colormetrics".

Offline faksuo

  • He is Risen! Our Forum Messiah!
  • Forum Spammer
  • Posts: 747
Re: Methcathinone - cold reaction w/KMnO4
« Reply #10 on: November 23, 2006, 02:25:41 am »
The reaction using bleach doesn't work either.  It turns the whole lot into benzaldehyde.
still in machine-like stride

Offline you

  • Even More Contributor
  • Posts: 167
  • At least I tried
Re: Methcathinone - cold reaction w/KMnO4
« Reply #11 on: November 23, 2006, 10:01:11 am »
All these stuff was written for ephedrine not for pseudoephedrine.

Anyways. If you got pure (pseudo)ephedrine then make meth.


cheers
Using drugs is legal where I live, possession of small amounts is a misdemeanor.

Offline Dr. Faustus

  • ubergeek
  • Lycaeum Addict
  • Posts: 1995
Re: Methcathinone - cold reaction w/KMnO4
« Reply #12 on: December 03, 2006, 08:32:32 pm »
Quote
There has not been too much talk about cat of late. Whatever the case, this thread could really be transferred to the Den.

Feel free to send it on over, if you'd like.
"I feel more like I do now than I did when I got here!"

~Uncle Dave~

Offline DrYRHead

  • Uberator
  • Ultimate Contributor
  • Posts: 9529
  • Sally as the cave
    • http://www.elfstarstudios.com/rabbit-hole.html
Re: Methcathinone - cold reaction w/KMnO4
« Reply #13 on: December 05, 2006, 01:19:42 am »
The reaction using bleach doesn't work either.  It turns the whole lot into benzaldehyde.

Yes, bleach(NaOCl) destroys amines, and turns them into ammonium chloride or related stuff.
DrYRHead

Welcome to the rabbit hole.

Offline DrYRHead

  • Uberator
  • Ultimate Contributor
  • Posts: 9529
  • Sally as the cave
    • http://www.elfstarstudios.com/rabbit-hole.html
Re: Methcathinone - cold reaction w/KMnO4
« Reply #14 on: December 05, 2006, 01:33:45 am »
All these stuff was written for ephedrine not for pseudoephedrine.

Anyways. If you got pure (pseudo)ephedrine then make meth.


cheers

 LOL yes, meth is stronger and lasts longer then cat. Either ephedrine or pseudo' can be oxidized into cat or reduced into meth, so most cooks that started out cooking cat changed to cooking meth. At least that is what has been said to have came to pass in the upper peninsula of Michigan.
DrYRHead

Welcome to the rabbit hole.

Offline Volatile

  • Contributor
  • Posts: 90
Re: Methcathinone - cold reaction w/KMnO4
« Reply #15 on: December 08, 2006, 01:17:18 am »
I don't know about easier... This reaction requires snapple bottles, coffee filters, a drying pan, and a precursor that is given to you in modest quantity in any first year chem lab. If you use dilute hcl instead of conc you would have to be WILFULLY FUCKING STUPID to hurt yourself.

And any tweakers who have ever let a RI/P rxn get too hot can attest that the same is not true of meth synthesis.

(and the dichromate method is potentially toxic)
« Last Edit: December 08, 2006, 01:19:08 am by Volatile »

Offline DrYRHead

  • Uberator
  • Ultimate Contributor
  • Posts: 9529
  • Sally as the cave
    • http://www.elfstarstudios.com/rabbit-hole.html
Re: Methcathinone - cold reaction w/KMnO4
« Reply #16 on: December 08, 2006, 12:38:43 pm »
Yes, dichromate is a carcinogen, :evil: and the Jone's reaction also uses pure H2SO4. :-o That does, indeed, make that reaction more dangerous than the cold reaction ( KMnO4+H2O).  :roll:
DrYRHead

Welcome to the rabbit hole.

prolixity

  • Guest
Re: Methcathinone - cold reaction w/KMnO4
« Reply #17 on: December 08, 2006, 01:46:56 pm »
Yes, dichromate is a carcinogen, :evil: and the Jone's reaction also uses pure H2SO4. :-o That does, indeed, make that reaction more dangerous than the cold reaction ( KMnO4+H2O).  :roll:

Swern method would work wonderfully if one doesn't mind the dimethyl sulphide.

prolixity

  • Guest
Re: Methcathinone - cold reaction w/KMnO4
« Reply #18 on: December 08, 2006, 01:52:16 pm »
appears one could do away with the DMSO even.. 

Readily available 6-(methylsulfinyl)hexanoic acid (1) is employed as a substitute for DMSO in Swern oxidation reactions using oxalyl chloride to smoothly convert primary or secondary alcohols to corresponding aldehydes or ketones in high yield. The resulting 6-(methylthio)hexanoic acid (2) is easily separable by aqueous extraction or by filtration through silica gel and can be reoxidized to 1 with sodium metaperiodate in 97% yield. Low temperature (-60 C) 13C NMR spectrometry is used to examine the intermediates of this Swern process. The results indicate that any residual unoxidized alcohol is generated during Pummerer elimination of the alkoxysulfonium intermediate and can be minimized by extended exposure to triethylamine at -40 C. Reaction of the potassium salt of 1 with cross-linked chloromethyl polystyrene affords a polymer-bound reagent 12 that quantitatively oxidizes borneol to camphor when used in two-fold excess.

Offline Dr. Faustus

  • ubergeek
  • Lycaeum Addict
  • Posts: 1995
Re: Methcathinone - cold reaction w/KMnO4
« Reply #19 on: December 08, 2006, 02:24:25 pm »
Quote
Yes, dichromate is a carcinogen,  and the Jone's reaction also uses pure H2SO4.

Of course, anyone who can't work safely with H2SO4 probably should not be doing any synthesis.
"I feel more like I do now than I did when I got here!"

~Uncle Dave~

Offline Dr. Faustus

  • ubergeek
  • Lycaeum Addict
  • Posts: 1995
Re: Methcathinone - cold reaction w/KMnO4
« Reply #20 on: December 08, 2006, 02:37:32 pm »
Quote
Swern method would work wonderfully if one doesn't mind the dimethyl sulphide.

Thanks. That is a very useful transformation.

http://en.wikipedia.org/wiki/Swern_oxidation

I like the variation at the bottom using TFA anhydride.

Below are several other variations that offer differing conditions, in the event that other functional groups within the molecule are susceptible to reaction under Swern conditions.

http://en.wikipedia.org/wiki/Corey-Kim_oxidation

http://en.wikipedia.org/wiki/Pfitzner-Moffatt_oxidation

"I feel more like I do now than I did when I got here!"

~Uncle Dave~

pylkko

  • Guest
Re: Methcathinone - cold reaction w/KMnO4
« Reply #21 on: December 09, 2006, 04:31:59 am »
Is there some idea, ref or something on why the sodium hypochlorite version would not work?

Offline Volatile

  • Contributor
  • Posts: 90
Re: Methcathinone - cold reaction w/KMnO4
« Reply #22 on: December 12, 2006, 12:37:09 pm »
I think that hypochlorite COULD work. The problem is that it is a much stronger oxidizer than KMnO4, and one would likely have to adhere to much more specific reaction conditions in order to prevent yields of all (Phenylmethylene)-methylamine and benzaldehyde.