Update: After chilling the xylene, a MOTHER LOAD of white crystals started growing on the glass walls of the distillation flask:



I am afraid these "crystals" are likely just MgSO4 precipitates

So therefore I will proceed with separation of the solids and the brown liquid, this will be dried as much as possible and washed with acetone.

The rest will be chilled overnight at -18 °C to see if no more precipitation happens.

Rady to filter:



Filtered white precipitate on sintered funnel:



Remaining precipitate in the distillation flask. You can see some sticked onto the thermometer adapter as well:



Flask with trapped MDMA.HCl on bottom. It hardened pretty well:



Scraped white precipitate, most likely just MgSO4:



I don't know how could MgSO4 dissolve in such high amounts (maybe I should dry the alcohol and xylene separately, filter each and then mix them. I poured the dry IPA in the xylene while it had MgSO4 still in it, so that might caused it dissolving in the mixed solvent).

The bottom layer (supposedly MDMA.HCl) hardened to the point it's impossible to scrape.

I think the course of action would be to add xylene and heat the flask in a hot water bath, until all the drying agent redissolves in the xylene, then simply decant it and give the flask few washes with fresh xylene.

Finally, the bottom layer should liquify too, so it would be possible to pour it in a Pyrex dish for drying. Then it will be broken, scraped, washed with acetone and finally dried.

Okay the project was somewhat successful.

The bottom MDMA layer in the RBF hardened overnight and stayed stuck to the glass and was sorrounded by MgSO4. I put the flask still with xylene in in a hot water bath (90 °C). This dissolved all the precipitated MgSO4 into the xylene and as a bonus, the MDMA layer popped off the glass wall by the mere action of swirling the flask.

I crushed it into smaller pieces and poured it through a filter. Then collected the MDMA rocks in a mortar (5.6 grams wet weight):



I crushed it, spread in a Pyrex dish and left outside to dry from the xylene:



Finally, I returned it to the mortar and gave it three cold dry acetone washes.

I transferred the wet powder in a Petri dish (leftover material was washed from the mortar with fresh acetone) and put the dish on a hotplate set at low, which fan blowing air over it, while mixing it with a spatula. This quickly removed most of the acetone:



Finally, I powdered the MDMA again in a mortar and transferred to a vacuum dessicator in a Petri dish, to remove traces of solvents:



Assuming the original MDMA content was 10 000 mg, I assume the yield will be in the 40-55% range, which is acceptable provided that I did this for the first time.

The lessons learned and improvements for anyone who would need to salvage MDMA dissolved in water:

- wash with NPS (DCM, toluene, xylene)
- dilute with distilled water, so the MDMA.HCl concentration is not too high (say below 25 mg/ml)
- base with NaOH solution (pH 12-13 ?)
- extract with DCM
- evaporate the DCM to get MDMA oil (distill off in a water bath or rotavap)
- prepare solvent mixture (dry toluene/xylene with dry IPA - 3:2 ratio)
- dissolve MDMA oil in a minimum amount of solvent
- add concentrated HCl drop-wise, regularly mixing and checking pH until the solution stays acidic (pH 5-6)
- distill off the IPA and water fractions until crystals will crash out from xylene
- chill the distillation flask
- filter the content, collect MDMA.HCl rocks
- dry, wash with cold dry acetone, dry
- for extra purity optionally recrystallize from dry IPA (see BOOFF Tek)

There is likely still MgSO4 in your product, MgSO4 does not dissolve in xylene even if its really wet. Those crystals were either your product or something else, my guess it was the product! If you have reagents around its useful to do the colour drop test to see. OR you can do the ever reliable bitter or salty taste test.... but you didn't hear it from me!

I don't know how much MgSO4 got in, but always filter the extracts after you dry them so that you have a clean transparent solution before doing the acid titrations. Also, I recommend using potassium carbonate as a drying agent instead of MgSO4, it works better, is easier to filter, and MgSO4 can interact with the freebase amine.

I would recommend you perform a recrystallization to remove the MgSO4. You can dissolve it in boiling anhydrous IPA, decant from insolubles, cool to crystallize and can add anhydrous acetone and place in the freezer to push everything out.

It could be something from the MgSO4 as the chemical supplier sells it as food grade (for dietary purposes) but it should be high purity as well. Now thinking about it, maybe I should have purchased real lab grade MgSO4... Another possibilty is CaCl2 I used earlier for drying IPA, also filtered but not distilled.

The stuff must have dissolved since the solution was really clear and transparent after filtering through 2 stacked paper filters and glass sinter (though the filter paper has not perfecly covered the sinter).

OK I will label the product as crude and continue with purification later.

Thanks for the boiling IPA tip.

You shouldn't dry alcohols with CaCl2, it can form complexes with them that remain as liquids. So its possible you got some calcium salts in there.

Food grade MgSO4 should be no problem, espom salts too, its all pure MgSO4. MgSO4 shouldn't even be fine enough to go through a sinter, if it was clear and transparent before you added the acid then everything should be fine, I think you might just be mistaking the product for it. Unless its from something else. Seems all fine to me I think the problems were all just related to the water content.

Re crystallization with IPA and acetone will remove the brown colour and provide you with real crystals. Definitely dilute the IPA with dry acetone after it cools down because even freezer temp IPA can keep the hcl salt dissolved, so dilute it a bit with acetone before putting it in the freezer, 50:50 even.
I like to collect these using a small sinter but paper works fine too. Always do some form of crystallization before washing with dry acetone, otherwise the washings are ineffective because the powder/paste can trap the brown impurities.

Okay. Following Mindlusion's advice, I proceeded to purify a part of the substance in question.

All glassware was flame-dried and all solvents were dried with anhydrous magnesium sulfate.

I loaded 895 mg of the powder in a 250 ml RBF:



Here is my reflux setup. The heat source is near boiling water and the coolant is iced water:



I have added few milliliters of IPA and waited until boil. It required few more milliliters of IPA until everything dissolved:











A precipitate shown up soon after leaving the solution to cool:





After swirlign however, this looks more like salt impurities:



I realized I forgot to add acetone to the IPA so I returned it to reflux and added some (3 ml or so). I haven't managed to bring the solution to boil. Probably due to evaporative cooling from acetone, preventing the mix to reach b.p.

I filtered the solution and transferred to a crystallizing dish, heated and evaporated some of the liquid:



I dosed the IPA with some more acetone as most could have evaporated.

Finally, there was only small amount of somewhat thick, syrupy brown liquid. I transferred this to a fridge waiting for any crystals appear:







I scraped the dish with glass rod and will see tommorow.

Interesting to see how this is progressing - I hope you haven't thrown anything away yet, b.m!



MgSO4 tastes pretty bitter too, although I'd say it lacks that special tang that MDMA has

Okay crystals appear. Could it be MDMA hydrochloride? I was looking around the net and cannot find a decent photo of the crystals under microscope to compare the structure.

I really hope I am not crystalizing impurities, like some sugar from the juice ...

Many people here have a crystal fetish, so here is the closeup to please your eyes



In the end, I will do a Marquis test to be sure. Maybe also on the impurities, but I am afraid the test is so sensitive it will react positively in every case.

I have finisehd the recrystallization today so here is the final report:

After two days in the freezer, the dish looks like this:



I washed the crystals off the surface with cold dry acetone (they gave up easily) and poured everything through a paper filter disc. I washed the glass dish and the filter with more acetone.

When adding acetone to the residual liquid, a observed clouding which signifies there is some product left over in the IPA/acetone mix:





I scraped the crystals carefully off the filter, vacuum-dried (over CaCl2) and weighed. The scale reads 576 mg:



This is 64.3% of the original amount, so assuming this is somewhat pure MDMA, we have bottom bound on the purity (provided there were some inherent losses, I therefore guess a minimum of 65-70% purity).

I dried the residue in the open air, then using a hair dryer. I remained as brown-ish oily syrup. I tried to scrape it with razor, and to my surprise, it solidified upon scraping into grey-white wet solid weighing 375 mg:



My hypothesis is that the residue still contains quite a bit of crystals since it crystallized upon the sraping.

I will try acetone washes on this to see how much remains.

There is one problem though: The total weight (product + residue) is 951 mg, which is 56 mg MORE than the source material. So either something got in during washing/re-x (less likely) or the residue still contains some IPA/acetone (more likely) or MgSO4 went through (CaCl2 is now out of game as I used fresh solvent from the bottle).

One more look on the final product:



Here is the product and the residue side by side:



Now I really miss my Marquis reagent. I will make some during the week just to test the substance. But at this point I am quite confident this is MDMA as it behaves exactly as it should against the solvents.

It is still possible I have crystallized magnesium sulfate as the salt forms similar crystals.

The residue is insoluble in acetone, but immediately dissolved in IPA, making it greyish-light-amber in colour.

I've added generous amount of acetone in the IPA solution and put it to the freezer. Maybe something will crash from it.

Fantastic work.

I'm off to the supermarket to buy all the blueberry juice I can just to see how much MDMA can be extracted from it /jk


(New Urban myth in the making?? )

Ha ha. Yes - I told my girlfriend that I extracted MDMA from bluebery juice and she said "You're na alchemist!!" ... well she also though the juice was a relevant precursor ... so I explained it wasn't such a big deal.

Well you can still make MDMA from such mundane items as cloves, almonds or even black pepper (next: Making M from almond milk )

The taste test definitely confirms bitter-soury MDMA taste, nothing like MgSO4. So what remains is Marquis to definitely confirm it.

yep

I know



Wake up and smell the lilac!