MDMA freebase --> MDMA.hcl via titration

[Potential]

Assuming one has A/B extracted, distilled freebase...gasses it (in dry xylene) using a HCL gas generator...saves the gassed xylene and washes with an HCL solution...then seps off the water layer...reduces the water layer until crystals being to appear...washes with ice cold, dry acetone...tosses in freezer...filters and washes crystals...

Is there anything else those crystals could be other than MDMA.hcl???

The crystals have a "saltier" taste and less of an odor than MDMA.hcl crystals precipitated with HCL gas...

[MDMA_AcTIvEsTS]

YOU Just ANSWERED your own question..

The above described is correct.. there will be negligent purity contamination governed by the implication of purity steps taken through out.. As long as you have followed correct procedure then you should recieve a considerable pure product.

There will always be a minor amount of impurity' found in the final product.. however, this is only consistant with the purifications processes and TLC taken in the production procedures'.

The post that you have posted, needs little to be desired for, in a sense, fellow bees can point out possible contaminats, however that info is only useful if one can identify the contaminants themselves.

Might i suggest that you read more on possible contamiants in the production of MDMA before posting a question that is broad in its stance.

From a fellow be to another, this is merely a suggestion of kindness.

READ....READ....READ....READ....READ....  as the answers are all around us!

[nitrous351]

Potential, I don't understand your post... if you had MDMA freebase dissolved in some dry xylene, and you gassed it with HCl, you should have had MDMA.HCl crystals precipitate at the gassing. Are you saying you gassed and didn't get any crystals?
I also don't understand why you washed the post-gassing xylene with a HCl solution...

[Potential]

Nitrous...
I felt that my gassing procedure was not very efficient.  I did get a decent crop of MDMA.hcl from gassing, but I wanted to be certain I got it all...plus I wanted to try this titration procedure...judging from the pile of crystals after the titration, it seems that my gassing procedure was average at best...I just wanted to know if that post-titration crystal mass could be anything other than what I so hope it is (ie MDMA.hcl).  Perhaps a bioassay is in order...

[nitrous351]

is different than gassing. SWIN has never titrated before, but I know it's different than gassing (obviously). Even though I don't know much about titrating, I know you're going to have to provide more information than you have.

[Flippie]

Hi Potential,

I liked to read your post since the same question popped up in my mind some time ago. I don't know the answer yet but reading MDMA_AcTIvEsTS's reply make me think I know the answer now.

If your are using HCL gas and make very fine bubbles then you have a very good contact of the gas molecules with the freebase and the salt will come out of solution with a minimal amount of HCl used. [I think the better you disperse the bubbles the less volume of gas you need for making the salt since the finer the bubbles the higher their specific surface is]

Of course adding a huge amount of HCl by titration will also form the salt but your environment will contain much more HCl than with the gassing procedure. This could explain the saltier taste, since your MDMA.HCl crystals are contaminated with the excess HCl in solution.

I think it might be interesting to use very pure HCl if you do the titration to have no other contaminants than HCl in your final product.

If you do the titration with HCL, couldn't you wash the salt afterwards to get rid of the excess HCl?

I don't know if the above is correct, since it is just some of my reasoning

   

[MDMA_AcTIvEsTS]

IMHO opinion regardless of the way you end up with the final product it is negligable to determine to level of HCL in the final product. However, if your product turns a yellowy color then you have gassed to far, however this may be removed via recrystalization. To be able to determine the amount of HCL one is governed by the observation factor of crystalization.

The best procedure is to titrate with small amounts andlikewise with the HCL gas technique, therefore there is no overkill on the final crystalization step.

Keeping an eye on the final product in terms of color. remembering also that they may also be other impurities with in the final salt product.. therefore recrysalization being a must...

As purification is a MUST...

[cublium]

Cub gasses his solution til he can smell HCl coming out of the NP/amine solution.If there are any freebase amines left,the gas stays in solution,when all amines are gassed out,HCl doesn't stay in NP solution anymore and you can smell it.

[biffman]

SWIM has found that often when HCl gassing, not all of the product will be converted to the insoluble crystals.  One solution is that after filtering off the formed crystals make sure that no more form (place in freezer for a while and gas again to be sure) you can always distill off the solvent (xylene in this case) and any remaining product will come out as it approaches dryness.  However there may still be some impurities in them so usually if you was them well with clean solvent that should take out the solvent soluble impurities and the crystals should remain.  For some reason quite often a significant amount of the product is difficult to crystalize with the first gassing and if you aren't careful you will lose a lot of the product by disposing of the solvent not knowing that there is still product remaining in it