Recrystalling Methylone

[Cuban]

Currently, I have some fine white powder Methylone that I'm attempting to recrystallize for purity's sake.

My initial attempt (kitchen setup) was a shot glass in a pan of water. I poured 70% IPA into the shot glass, then heated the setup until IPA began to boil. I added 1g of Methylone, stirred, then added a small amount of IPA to completely dissolve the Methylone. I left the setup on LOW LOW heat to evaporate the IPA without heating too much the Methylone.

As the IPA evaporated, the solution became more and more yellow, with a few crystals beginning to form, very small however. It should be completed by tonight and I'll post results.

In the mean time, can anyone make suggestions for a better home set up/procedure? Also, since Methylone is a better solute in polar solvents, can someone suggest a safe, nontoxic nonpolar solvent? Preferably one whose boiling point is below Methylone's.

 

[sekio]

Recrystallizations must be done with high-purity solvents. Don't even bother with 70% IPA.

You're not even doing a recrystallization. Adding IPA and evaporating it isn't going to do shit all and in fact will wreck the purity of your IPA with the stabilizers and shit that are in rubbing alcohol. Go read up on recrystallizations and buy some 99% or better alcohol and then come back. Don't expect an amazing yield, either.

http://chemistry.about.com/od/chemistryhowtoguide/ss/recrystallize.htm

 

[23536]

I added 1g of Methylone

may I suggest you do this backwards. Add the hot solvent to the solute via a dropper or whatever

 

[23536]

will wreck the purity of your IPA with the stabilizers and shit that are in rubbing alcohol. Go read up on recrystallizations and buy some 99% or better alcohol and then come back. Don't expect an amazing yield, either.

stabilizers? Label in the US says the only other ingredient is water. Maybe the label isn't exhaustive

99% ethanol will have entrainers like benzene in it. Don't know if this'll affect the process. I've used 95% ethanol in the lab before with acceptable outcomes.

 

[Cuban]

stabilizers? Label in the US says the only other ingredient is water. Maybe the label isn't exhaustive

99% ethanol will have entrainers like benzene in it. Don't know if this'll affect the process. I've used 95% ethanol in the lab before with acceptable outcomes.

The dropper idea sounds great.

I'm not going to use water or an alcohol for further trials, as Methylone is too soluble in polar solvents, e.g ~358 mg/ml for H2O.

I've thought of using d-limonene, but I believe it's BP is higher than Methylone's. Could you suggest another?

 

[sekio]

Methylone doesn't boil at 1 atmosphere, it decomposes. And you shouldn't be evaporating the solvent off at all. The whole purpose of recrystallization is to grow pure crystals in the solvent, leaving impurities and a small amount of the original substance in the solvent and removing the crystals via filtration.

 

[Cuban]

Methylone doesn't boil at 1 atmosphere, it decomposes. And you shouldn't be evaporating the solvent off at all. The whole purpose of recrystallization is to grow pure crystals in the solvent, leaving impurities and a small amount of the original substance in the solvent and removing the crystals via filtration.

That is recrystallization with mechanical filtration. My procedure is closer to vacuum filtration, minus the vacuum. Essentially, a supersaturated solution is made in an unfavorable solvent and then quickly cooled and evaporated. This produces a purer, isolated product, but is typically powdery. Fast and hot procedure is a more powdery product while slow and low is a more crystalline product.

For lack of vacuum, I'm using gentle heat in attempt to allow crystallization while speeding evaporation time.

Recrystallizations must be done with high-purity solvents. Don't even bother with 70% IPA.

You're not even doing a recrystallization. Adding IPA and evaporating it isn't going to do shit all and in fact will wreck the purity of your IPA with the stabilizers and shit that are in rubbing alcohol. Go read up on recrystallizations and buy some 99% or better alcohol and then come back. Don't expect an amazing yield, either.

http://chemistry.about.com/od/chemistryhowtoguide/ss/recrystallize.htm

Minus your complaint about the solvent, I am doing a recrystallization. I increased the solubility of a solvent with heat to supersaturate the solution at STP, then am slowly removing the solvent, allowing the Methylone molecules to crystallize at the bottom and sides. I have crystals, albeit smaller than I imagined.

I have heard that polar solvents will degrade methylone after some time in solution, but the source wasn't credible. I don't know if that's happening, but I don't intend on using water in future trials.

A few hypotheses I have to improve the procedure are a wider vessel and a less polar solvent. A wider vessel will mean smaller crystals, but a faster procedure. A nonpolar solvent will ensure it falls of solution faster, allowing larger crystals. Some compromise between the two will need to be found. This is a home setup, so what I can do is limited. However, I already have a rudimentary knowledge of chemistry (A's in gen and orgo chem at a top science school), rather than a 'shake and bake' 'chemist.'

So, to match your complaints, can you suggest worthwhile improvements?

 

[vecktor]

That is mechanical filtration. My procedure is closer to vacuum filtration, minus the vacuum. Essentially, a supersaturated solution is made in an unfavorable solvent and then quickly cooled and evaporated. This produces a purer, isolated product, but is typically powdery. Fast and hot procedure is a more powdery product while slow and low is a more crystalline product.

if it is cooled and evaporated where do the impurities go? the procedure is generally called crashing out of solution and no it does not generally give the best purity.

standard practice for recrystallization is dissolve the solids in as little almost boiling solvent as possible, you do this by adding almost boiling solvent to the solids heating to boiling, if solids remain add a little more solvent, heat to boiling again filter quickly and then cool slowly. rule of thumb is start with 5 ml of solvent per gram of solid and add more.
don't evaporate the solution to get the first crop instead cool to 5oC and wait. filter off the solids, to get a second crop then evaporate the filtrate/ mother liquor until cloudiness at just under the bp of the solvent then add a little more solvent and then cool as before. the solids must be filtered from the mother liquor because the mother liquor contains the dissolved impurities, evaporating it just leaves the impurities mixed in again.

using 70% IPA is a problem because as you evaporate it, it forms an azeotrope with water containing 87% IPA so you lose more IPA than water and eventually you end up with mostly water. using 99% IPA is better. alcohols are perfectly suitable for recrystallizing methylone

the theory and practice of recrystallization is out there on teh interwebs probably a youtube video too,
suggest you take a look

Minus your complaint about the solvent, I am doing a recrystallization. I increased the solubility of a solvent with heat to supersaturate the solution at STP, then am slowly removing the solvent, allowing the Methylone molecules to crystallize at the bottom and sides. I have crystals, albeit smaller than I imagined.

I have heard that polar solvents will degrade methylone after some time in solution, but the source wasn't credible. I don't know if that's happening, but I don't intend on using water in future trials.

A few hypotheses I have to improve the procedure are a wider vessel and a less polar solvent. This is a home setup, so what I can do is limited. However, I already have a rudimentary knowledge of chemistry (A's in gen and orgo chem at a top science school), rather than a 'shake and bake' 'chemist.'

So, to match your complaints, can you suggest worthwhile improvements?

 

[23536]

Cuban, you may be fine with IPA or ethanol (honestly I've never worked on MDPV) but it sounds like you're not performing a couple of steps. Add only just enough hot (hot) solvent to dissolve everything, then let it cool at its own pace, then maybe lower the temperature even more with an ice bath, then filter

sometimes scratching the walls can help. Like here:

http://www.youtube.com/watch?v=amTAuK25P6c#t=7m05s

 

[Cuban]

Cuban, you may be fine with IPA or ethanol (honestly I've never worked on MDPV) but it sounds like you're not performing a couple of steps. Add only just enough hot (hot) solvent to dissolve everything, then let it cool at its own pace, then maybe lower the temperature even more with an ice bath, then filter

sometimes scratching the walls can help. Like here:

http://www.youtube.com/watch?v=amTAuK25P6c#t=7m05s

Thanks, I appreciate it. I'll try it both with a quick cool and a gentler cooler with pure ETOH (>99%) and see how they turn out. By the way, I'm working with bk-MDMA, aka methylone.

if it is cooled and evaporated where do the impurities go? the procedure is generally called crashing out of solution and no it does not generally give the best purity.

standard practice for recrystallization is dissolve the solids in as little almost boiling solvent as possible, you do this by adding almost boiling solvent to the solids heating to boiling, if solids remain add a little more solvent, heat to boiling again filter quickly and then cool slowly. rule of thumb is start with 5 ml of solvent per gram of solid and add more.
don't evaporate the solution to get the first crop instead cool to 5oC and wait. filter off the solids, to get a second crop then evaporate the filtrate/ mother liquor until cloudiness at just under the bp of the solvent then add a little more solvent and then cool as before. the solids must be filtered from the mother liquor because the mother liquor contains the dissolved impurities, evaporating it just leaves the impurities mixed in again.

using 70% IPA is a problem because as you evaporate it, it forms an azeotrope with water containing 87% IPA so you lose more IPA than water and eventually you end up with mostly water. using 99% IPA is better. alcohols are perfectly suitable for recrystallizing methylone

the theory and practice of recrystallization is out there on teh interwebs probably a youtube video too,
suggest you take a look

Thank you. Great post.

Are you suggesting filtering while hot to remove insoluble impurities? I didn't get that part. I understand cooling it to have methylone come back out of solution then mechanically filtering, repeat.

For the second crop, are you adding solvent to redissolve impurities, so they don't come out when cooled again?

 

[vecktor]

Thanks, I appreciate it. I'll try it both with a quick cool and a gentler cooler with pure ETOH (>99%) and see how they turn out. By the way, I'm working with bk-MDMA, aka methylone.



Thank you. Great post.

Are you suggesting filtering while hot to remove insoluble impurities? I didn't get that part. I understand cooling it to have methylone come back out of solution then mechanically filtering, repeat.

yes, a quick filtration, there shouldn't be a lot of insoluble crap but who knows with current RC's

For the second crop, are you adding solvent to redissolve impurities, so they don't come out when cooled again?

no, just concentrating the filtrate. if the impurities are fairly low concentration they stay in solution and the second crop is as good as the first, but if they are in high concentrations then the second crop will be worse quality than the first.

 

[dg420]

another neat trick is, find one solvent it is soluble in,(water, ethanol) and another it isn't(acetone, mek) and do the dual solvent crystallization
yields are a little lower, but the quality is tops

 

[SmokeaJoint]

Now, I'm about halfway through this thread, will be done reading before anyone replies. What I wanna know (so I don't have to make another thread) is, could I re-crystalize using pure acetone? I'm fresh out of 99% iso, my usual go-to solvent.

 

[mysticgreen]

be sure to use high quality aceton, lab grade aceton is usually used for washing and contains other solvents.


in principle aceton should work, but the recrystalation can be cumbersome, because i would expect the aceton to dissolve a lot of the methylone. you might need cooling (ice/NaCl or ice/CaCl2) might do the work)


good luck.

 

[atara]

Make sure that any solvent you use is clean by boiling some down first. If boiling a shot glass full of your acetone (no solute) leaves behind visible residue, it's probably not clean enough to use.

 

[Iodjini_dk]

^^It could still contain volatile impurities.

Alternatively, you could distill your solvents to obtain a higher grade. But that can be a little dangerous if youre doing it in your kitchen.

 

[SmokeaJoint]

Lets say for argument's sake that the acetone I have is 100% acetone with no additives. I haven't confirmed that completely, but evaporating a bit on a mirror showed no streaks or residue. So I'm guessing its pretty clean. I got it from the hardware store if that means anything.

 

[kong]

Being devils advocate but do you have any real reason to believe purity will be increased by recrystallizing? I've been told crystal methylone is made strictly for aesthetics as the powder or tiny crystal mixes are already very high purity. Unless you have reason to believe otherwise I'd leave it alone.
Crystal=slightly off white powder=tiny crystal mix ime...

 

[SmokeaJoint]

I have reason to believe mine got cut with.... something. I didn't order lab or supplier direct. Street methylone ftw.

 

[SmokeaJoint]

I think it came up earlier, or maybe I saw it on another site. I saw some cool freebase crystals last night of someone who was extracting pure coke from coca leaves. Little crystaline trees of freebase, so pretty. Sorry. off topic.