Crystallization of mdma oil in toluene.

[katsogiannos]

In reference to Placebo's RP/I reduction of ephedrine meth synthesis, meth freebase oil in toluene, will be crystallized by adding distilled water, and acidifying with hcl/muriatic acid until PH is 7. This way you don't have to run hcl gas through the toluene, although it is more tedious and you have to shake,test,add more HCL until you reach the right PH, and you have to be more careful evaporating the water so you don't lose some crystals.

My question is whether this same method will work for getting MDMA crystals. In methylman's reductive amination of MDP2P with nitromethane and Al/Hg, he seperates the water/sludge layer from the MDMA oil layer using toluene. The synthesis calls for anhydrous conditions, and since my chem knowledge is very limited, I am not sure if adding a little bit of distilled water, and acidifying with HCl, and evaporating the water to get MDMA crystals would work?

All inputs are greatly appreciated.

[terbium]

I have done this with meth and it works well but MDMA is more sensitive to heating in strong acid as this can cleave the methylenedioxy group. The problem is made worse because when you concentrate a solution containing just a little excess of HCl the water will leave first and the HCl will stay behind in the solution so that when you get down to the last bit of water it is a strong acid solution. If you go this route with MDMA you will probably want to either insure that there is a bit of excess, unneutralized freebase and/or take off the last bit of water at a low temperature like in a vacuum desicator.

[katsogiannos]

[Cept]

see if you can make some sense of this.
   from what i have noticed in visions, it's kinda cool to note that when evaporating hcl + h20 + freebase MA, the excess water that evaps doesn't leave too many xtals on the pyrex (dilution considered), it's only when the vapor stinks like hcl that lots of xtals dry on the glass.
  maybe the product prefers acid over water, even though they mix, and hcl comes off first (i dream of hot steamy evapping, and swear both come off simultaneously). and/or maybe it's just the increasing concentration of ma liquid that delays the stals from making their full presence known until later on.
  and in the very end as soon as mean hcl is evaporating, there they are.  i'll bet MA.hcl is more soluble in hot hcl than hot h20, that's all i'm saying.

obviously excess acid isn't the way to go with methylene dioxies when heating to evap.

[scram]

"it's only when the vapor stinks like hcl that lots of xtals dry on the glass."

No, this is not true. You can have a ph 8 after adding your hcl and you will still get mass crystals, and acutally cleaner crystals. Bringing the ph down to 1 (polar) and 5 on the toluene pushes out the rest. However, your acidic layer become red when it hits below 5.

[Cept]

Thanks, that makes sense. But why red? What's the significance? Do acids (proton donors) redden a system, and bases (electron donors) make it bluer or is that just a funky coincidence i've been dreamin up.
   Dreamin, i'd noticed something to do with pseudo color impurities before a rp/hi, usually light pink, but redder(brownish) after the refluxing acid reduction.
   Or, pinkish pseudo becoming bluer (greener) upon oxidation with permanganate.
   Or, clear distilled safrole and saturated lye when refluxing in ethanol for isosafrole. Immediately bleeding blue into the interface and eventually red on the bottom, basification bluens the upper phase and reddens the lower.
   Or, the Birch being blue because it is basic.
   Is it me, or does increasing oxidative forces increase the blueness of the system?