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Strange formation of mephedrone?

delterp

Greenlighter
Joined
Jun 6, 2013
Messages
8
Hello (New here!),
As this is my first post I'd just like to say that I am by no means a biology or chemistry expert, my limit of chemistry was A-Level!

Anyway, I know nothing much about mephedrone, so I ordered some and when it arrived I did the usual acetone wash (either very little or nothing was filtered), and I always dissolve and evaporate crystals to make sure they reform properly to see if they're mixed or whatnot (I'm not asking for a substance ID).

Anyway, I've had 2 batches of mephedrone off different sellers and both were crystals though one was square crystals mixed with shard crystals, the other was just lumpy shard crystals. I dissolved both in water and let them evaporate naturally, after about a day and a half, the water looks to have evaporated entirely but it hasn't from what I can tell as the resulting solid is wet. Both solutions give a yellow solid with a smell similiar to urine but weaker and sweeter (as best as I can describe it, both sets of crystals had no determinable smell before dissolving), putting it on to filter paper and pressing it down makes the filter paper underneth become wet... Whatever solution it is does not seem to be water as even a small amount takes days to dry off.

So I am perplexed as to what is happening and why the solution isn't reforming into crystals, again I am not after a substance ID but I am wondering if anyone has tried this (maybe with the pre-ban mephedrone?) and has any idea what is happening, I'm assuming the chemical becomes unstable in water or reacts with one of the other things in the water (Note: I used normal tap water from a hard-water area, not distilled water) and thus changes to a different chemical, but if this is so, how do the labs that produce it get it into clear crystal form? I'm assuming they use some kind of solvent that evaporates fast and doesn't react.

I don't have any pictures of the substances but can take some (though they will be low quality :p) if anyone's interested in what it looks like.

Thanks for reading and greetings :).
 
I don't know a lot about mephedrone either, but I think it's quite unstable in water. I've also read a lot of complaints of people saying they accidentally got it wet and it turned into a yellow odorous sludge. I think you are right that one would have to use a solvent that evaporates quickly and doesn't react with it. Is there a reason that you can't use acetone to recrystallize? Maybe I'm missing something...

I want to move this somewhere where you will get better answers, as I don't think it's really a basic question. Maybe to Other Drugs... But first just to clarify, are you just looking for a way to roughly test whether the substance you have is likely pure, or a way to purify it? Or neither?

I found this study that found that mephedrone degraded at different rates depending on the pH of the water. After 12 hours in water at a pH of 7, 5% of it had degraded into by-products, and after 12 hours in water at a pH of 12, 65% of it had degraded into a by-product. I assume your water would be somewhere in between, since you said it was hard water.

I would also not use the yellow wet stuff because I have no idea if any of the degradation products are toxic or not.
 
The crystals don't dissolve in acetone nor IPA so I can't recrystalise using either.
I was doing it to purify it but after seeing it change yellow I thought it wasn't worth bothering with so it's just 'junk' I can mess around with really (both the crystals and yellow gunk).
That does look to be an interesting article, I'll give it a read tomorrow, thanks!

Interesting to see that it's really unstable, I wonder how quick it degrades just in air.
I would assume they possibly are, initially (before the ban) I don't remember any reports of 'blue skin' or muscle pains that came about near and after the ban so I would assume that they're probably likely partially responsible for them.
 
Oh I think maybe you have to heat the solvent to dissolve mephedrone in a solvent like acetone, ethanol, methanol etc? But I would not recommend a person without sufficient chemistry knowledge/experience heat those kinds of solvents at home though, sounds dangerous - definitely do thorough research on safety if attempting that. I am also not even clear on whether that would remove all likely impurities or not. I am guessing if mephedrone is only soluble in a given solvent when hot, you could use a process involving heat to remove any impurities that are soluble in the solvent when it's both hot and cold.

But by the same token washing the crystals in cold acetone should presumably remove at least some impurities. I am definitely no expert on this stuff, sorry :)

It's really hard to find any good info on this because it seems like, at least pre-ban, mephedrone was generally high purity and so there weren't many users desiring to put effort into purification. I can't really find anything other than these 2 threads:

"Purifying 4-mmc". Which may not be much help - the guide nuke linked to in that thread looks advanced to me in spite of its name.

"crystallization". What seep says in this one kinda goes along with my idea above, but he doesn't fully explain the process (and it doesn't sound like he's actually used it for mephedrone).

*Please note that those 2 threads are old and might not give adequate safety advice or might assume the reader knows certain safety protocols.

I'm still not sure where to move this so maybe I'll just ask some other mods where they think it would get more responses.
 
I've tried to get these crystals to dissolve in cold and heated acetone - it won't dissolve in it at all.
I found some sulphuric acid lying around and added a bit of it to that and it fizzed and dissolved - I'm assuming it's reacted with it though, and I don't really have any safe way to evaporate the sulphuric acid. But from what I remember, similar reactions occur between hydrochloric acid (stomach) and sulphuric acid, so does that mean when it reaches the stomach it changes into another chemical?
I also added some lemon juice to acidify some water and dissolved some in that and it's in the final stages of evaporation so I'll check that later.
The double boiler method is also used with ketamine if it's the method I'm thinking of, though I've not heard about different 'cuts' being suspended at different points, still not sure about that. The extracting amines one is way too complicated for me haha.

OK, here are some pictures.
Crystals as they came in bag: http://i.imgur.com/lKgWyZk.jpg
Yellow substance from water evaporation (Note the 'dried in' yellow to the filter paper at the top-left, this was from another vendor which is purpotrated to be much weaker and had the 'grease' stain when put onto the filter paper): http://i.imgur.com/YT4ZKew.jpg
IPA-evaporation (I think the outside parts are all fine but probably from the traces of water in the IPA as it's years old): http://i.imgur.com/DLiBIb6.jpg
IPA-evaporation close-up: http://i.imgur.com/PiB6GWK.jpg
Acetone-washed (about 4 times) crystals (Note that there is some very slight yellowing of them): http://i.imgur.com/hg6KjKv.jpg
 
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I think the best thing would be to get a reagent test kit like the EZ Test Bath Salts test (I hate the name lol) which tests for mephedrone, methylone and MDPV. That way you could at least determine if it even is mephedrone that you have. Such a test can't tell you how pure it is but can at least detect the drug's presence. If it turns out it's not even mephedrone then ways of purifying or recrystallizing mephedrone won't work (not to mention for safety reasons it would be preferable to know!).

I'm going to move this over to Advanced Drug Driscussion, maybe they can give you some advice on the purification situation and if they want they can move it to Other Drugs.

BDD -> ADD
 
Haha thanks. I think I've given up with this anyway. The lemon water evaporated but has left lemon entangled with the chemical, tried doing the IPA double-boiler seperation but it didn't go too well, the resultant substance is sticky, dark yellow and smells mostly sweet with a slight sour undertone, which is pretty strange.
Seperation: http://i.imgur.com/ov6LPXc.jpg
Close up: http://i.imgur.com/Hv7Nkqx.jpg
The only test I've got left with it is the sulphuric acid one but I might just forget it seeing how much of a pain it'd be to evaporate it safely.

Unless anyone else can think of any other tests or 'fun' chemical stuff to do with it, I'll just bin it?
 
It seems to me the "wet" crystals are from either:
1. water entrained in the xtals... i'm not sure if mephedrone is hygroscopic, but i do know it will take AGES to dry completely at room temperature.
2. Mephedrone breaking down to 4-methylbenzaldehyde and methylamine and stuff (fish/urine/"pistachio"/"sweet" smells)

probably both.

The way you'd produce anhydrous crystals is by dissolving the freebase in e.g. isopropanol and gassing it with hydrogen chloride (or adding HCl in acetone) which causes the precipitation of mephedrone HCl. the labs probably don't bother recrystallising the hcl.

You can still take the gummy yellow shit, but expect reduced potency. I would personally bin all of this stuff and write it off as a learning experience not to get meph wet.

To recrystallise I would dissolve the meph in hot isopropanol and let it cool overnight.
 
I wouldn't think it's from water in the crystals, using the double boiler method dries the crystals out fully and still leaves them yellow, the breaking down would make sense though.
I've just been trying for a while to get the crystals to dissolve in hot IPA but it will not dissolve at all, so recrystalisation using an IPA solvent doesn't seem possible.
It's all written off, I had a small amount and got pretty painful limbs from it (it was dissolved in water so chances are it changed to whatever the yellow product is) so will not be having any more of it again, hence why just doing tests with it.
 
Color is really the worst way to asses the purity of your compound! A very low amount of impurities could give a strong color to the product.
Also, it's not improbable that a slightly white solid gives, once dissolve, a slightly yellow solution.

For the odor, it probably comes from triethylamine (or a similar amine base... or methylamine) which is sometimes used in the last step of the mephedrone synthesis (before the formation of the salt). This amine base should be in a salt form in your powder (and salt have no smell). Once dissolved in water, the amine base should get deprotonnated and then be more volatile and smelly.
This kind of amine are also sensitive to oxygen and oxidize slowly to give yellow-brown side-products.


Mephedrone breaking down to 4-methylbenzaldehyde and methylamine and stuff (fish/urine/"pistachio"/"sweet" smells)

It's not improbable, but I strongly believe that mephedrone is stable in water at room temperature.

On another subject, this washing/recrystallization appear to me a bite useless when we don't even know what are the impurities.
 
It's not improbable, but I strongly believe that mephedrone is stable in water at room temperature.

According to the study I linked above it is not generally stable in room temp water. How fast it degrades greatly depends on the pH of the water. It was stable in very acidic water (presumably slightly acidic might be ok too), but it was not stable in neutral or alkaline water. In alkaline water it degraded rapidly.

Degradation products:
It also says the degradation pathways were as follows: (a) 4-MMC > MPPD > MBA > DMBA and (b) 4-MMC > N-Ac-4-MMC (In pathway (a), the first reaction is the oxidative deamination of 4-MMC to form MPPD; Methylamine would be produced at the same time).

[4-MMC = 4-methylmethcathinone; aka mephedrone]
MPPD = 1-(4-Methylphenyl)-1,2-propanedione
MMA = methylamine
MBA = 4-methylbenzoic acid
DMBA = N,4-dimethylbenzamide
N-Ac-4-MMC = N-acetyl-4-methylmethcathinone
 
Color is really the worst way to asses the purity of your compound! A very low amount of impurities could give a strong color to the product.
Also, it's not improbable that a slightly white solid gives, once dissolve, a slightly yellow solution.
The solution is completely clear, once evaporated, the substance left behind is yellow

For the odor, it probably comes from triethylamine (or a similar amine base... or methylamine) which is sometimes used in the last step of the mephedrone synthesis (before the formation of the salt). This amine base should be in a salt form in your powder (and salt have no smell). Once dissolved in water, the amine base should get deprotonnated and then be more volatile and smelly.
This kind of amine are also sensitive to oxygen and oxidize slowly to give yellow-brown side-products.
On another subject, this washing/recrystallization appear to me a bite useless when we don't even know what are the impurities.
I don't know what any of it is, the acetone wash was meant for removing cuts from the powder and the recrystalisation was to make bigger crystals.
Interesting.

Also n.b. the solution of sulphuric acid that had a sample added has now gone a red colour, I'm not really sure why.
 
To recrystallise I would dissolve the meph in hot isopropanol and let it cool overnight.
OK so I left the solution that had IPA and crystals in to dry, none of them dissolved but something pretty odd has happened; http://i.imgur.com/7PnBKFX.jpg
It's a bad pictures but at the bottom is a white solid (no longer clear as they originally were) with some tiny sparkly crystals (like the yellow powder), and at the top level of where the IPA was there's now some solid around there (the partial ring of what looks like reflective light in the picture, it isn't light and is indeed a powder), which doesn't make sense because all the crystals sunk to the bottom... So I'm once again unsure if it's broken down in IPA or what.
 
The IPA is evaporating and as it concentrates down, something (mephedrone) is precipitating out.

The crust around the rim is known as bearding.
 
The crust around the rim is known as bearding.
(Despite being off-topic) Is the same thing likely to happen with ketamine slowly evaporated from water (Again, hard tap water not distilled)? (Using a curved shot glass) it's left clear crystals from the middle downwards and white powder from the middle upwards. I tried dissolving the white powder in IPA and acetone and neither dissolved it, added it to sulphuric acid and it fizzed like the crystals do and finally did a aluminium foil 'burn/melt test', the powder went a dark red colour and the crystals (taking considerably longer) go to a much brighter red and there's much less of it than in the powder?
 
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