MDMA Crystals

[DiMethyl]

I am recrystallizing some MDMA and I am getting some very big crystals (slow growth).
Does anyone know what mdma crystals look like?
I am getting parallelogram shaped crystals.

[Rhodium]

It depends on the crystallization conditions, such as humidity and what solvent you use.

[DiMethyl]

The mdma crystal's properties should be dependent on the chemial properties of the mdda molecule.
Every crystallizaable compound has a distinct crystal shape and I would think that would not vary between solvents of crystallization.
Here is what I did:
I noticed that some mdma.hcl that had been sitting around for a few months had acquired a yellowish brown color.
Yuck.
I just did not feel too good about putting that up my nose.
So---I disolved the material in the minimum amount of hot 70% ipa and let cool.
No crytals at room temp so I put the beaker in the fridge.
Still no crystals.
I put them beaker in the freezer and the next morning when I got up and checked there was some rock salt looking crystals in the bottom of the beaker which bio-assayed very very well.
The liquid that was decanted from the rock salt stuff was put in a petri plate and allowed to evaporate over 3 days.
During this time some very large crystals grew.
I washed them with ice cold acetone and they are very clear.
I should bio-assay them and I will get back with the results.
DiMethyl

[fierceness]

Every crystallizaable compound has a distinct crystal shape and I would think that would not vary between solvents of crystallization.

That is completely wrong.  Check any source that has information on crystal type -- it usually says "forms <shape> from crystallization in <solvent(s)>".. each solvent or combination of solvents can form different crystalline structures.

[DiMethyl]

Those large crystals---up to .5 inch in length--bio-assayed as excellent.
So, I have found the answer to my original question.
I have a hard time believing that NaCl crystals look differnt when crystallized from h20 as opposed to crystallizing from Et-OH, but you may be right.
I'm no expert.
The slower the crystals grow---and the bigger they are---the more pure is the desired compound.
DiMethyl

[TheBlindGenius]

I would think some of your MDMA dissolved in the 30% water.  I would have used straight IPA, or at least drugstore 91%.  You must have lost a shitload.

[Rhodium]

MDMA forms a number of hydrates when crystallizing, depending on how much water is present (Ref: Pihkal #109), meaning that a varying number of water molecules are incorporated in the crystal lattice along with the MDMA molecules.

If you fill a box with oranges and shake them, they form a certain pattern, with them stacked neatly in layers (this corresponds to a pure MDMA.HCl crystal). If you add a few dozen ping pong balls (representing water molecules) to the mix and shake, the stacking pattern won't be the same any longer, and the overall crystal shape will also be different. Hence, the crystallization conditions will heavily influence the crystalline shape.

Also see the discussion in this thread about solvent effects:

Post 398077 (missing)

(GC_MS: "3,4,5-trimethoxynitrostyrene xtal shape", Newbee Forum)

[DiMethyl]

I took two of the large mdma crystals from the petri plate.
Each crystal was about 1/2"X1/4" and flat and as clear as window glass.
I proceded to crush these two crystals to produce two medium sized lines----which I did.
I have taken mdma many times but this was very different.
The high was very speedy and lacking the degree of emphatic effects usually manifested by mdma.
The high was fantastic and affected me more than any other mdma experience.
The duration was about 4 hours---but the effects still linger today----24 hours later.
During the high I remember thinking that perhaps I had inadvertenly done meth---but the one thing that came to mind was mda.
Now this leaves me wondering if a potential byproduct of  methyl man's variation of the bright star synthesis is actually mda?
When my hydroxlyamine.hcl arrives then I guess I will be able to determine the answer to that.
But----what I experienced last night with the large crystals was very different from my usual mdma experience.
Another explanation is that the large crystals were very very pure mdma.
That---perhaps---is more plausible.
DiMethyl

[hypo]

but the most plausible explanation is: placebo! resp. set & setting.

anyway, why does your MDMA.HCl get brown!? forget the MM writeup.
do an A/B and distill your freebase. (easier than distilling ketone)
no need for recrystallisation then...

(crystals are for pussies - get some CuSO4 if you want crystals   )

[abacus]

There is NO subsitute for distilling the MDMA freebase.  If you follow the MM workup your gear will go sticky and off colour over time.

It amazes me that distilling the freebase isn't a "must do rule" by now.

Abacus

[DiMethyl]

Yes---distilling the ketone takes me about 12 hours with the vac pump going full bore the entire time.
It actually does go fairly smoothly but it just takes a long time.
I have been reluctant to distill the mdma free base due to concern that I might fuck that up and lose all that work and product.
The mdma.hcl crystals at the beginning of the hcl gassing are snow white and they are not kept around for an extended period of time due to their popularity.
What is kept for longer periods are the last of the crystals produced during the hcl gassing phase.
I suspect that during this phase the initial crystals are quite pure and that it is only towards the end of the process that the impurities start to crash out with the mdma.hcl.
Regardless, I should distill the mdma just to note the difference.
Has anyone here done the distillation of the freebase and if so can you direct me to a writeup of the procedeure?
Of course I can use the search engine to see if I can find anything.
I will probably procede without a writeup of the procedeure but then all that product hangs in the balance.
DiMethyl

[Jackhammer]

Rhod, you´re completely right. At college when I analysed some MDMA.HCl batches I found differences in their IR spectra. After drying of some of those crystals the diferences disappeared. I think this was an example of water beeing incorporated into the crystal lattice.