FYI here's that article about the Indonesian lab. All thanks for Moriarty for this find:
The DEA Singapore Country Office and DEA Special Testing and Research Laboratory (Dulles, Virginia) recently assisted in the seizure of a very large MDMA/amphetamine operation in Tangerang, Jakarta, Indonesia. The laboratory was seized by the Indonesian National Police, andconsisted of a chemical synthesis laboratory and a separate tabletting operation. The synthetic route to MDMA involved reductive amination of 3,4-methylenedioxyphenylacetone (MDP2P or PMK) with methylamine and sodium borohydride; the hydrochloride salt was produced by gassing an acetone solution of the free base with commercial hydrochloric acid gas.
h**p://www.justice.gov/dea/programs/forensicsci/microgram/mg0103/mg0103.html <- be careful with that link
i do also recall the hive post "Processing 1 Mole Ketone Using Nitromethane" by Abacus who came up with the method of reducing nitro via the al/hg first, isolating the MeAm and then running a standard MeAm Al/Hg. Abacus was a big advocate of gassing in acetone, he distilled his freebase and use 4x v/v acetone to freebase. i know that doesn't say anything but i figured i'd toss it out there. here is the link to that post
http://127.0.0.1/rhodium/Rhodium/hive/hiveboard/methods/000382493.htmlFrom that same "Processing 1 Mole Ketone Using Nitromethane" stated above, Osmium came through and said "I can also recommend the following crystallization procedure: dissolve freebase in IPA, gas with HCl, and then crash out the product with excess acetone. Store at -20°C for some time and filter. Save those mother liquors, still some goodies in them!"
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Yeah Vesp there are quite a few possibilities depending on your technique, seems like a lot of different by-products that could be produced, some of them are crystalline and probably difficult to differentiate from your amine salts too. granted i'd imagine it would take more time than what's used in a simple gassing to obtain these by-products, it's just a really scary thought and personally i'm one that's big of piece of mind for knowing my solvent won't react to form something unexpected. at the same time i'm tired of tasting xylene/toluene. i had always worried IPA was too polar to work well for gassing MDMA HCl but maybe not? i guess it just depends on what the dielectric constant drops to at < 0C. it'd be great if someone had a reference for IPA's dielectric constant at 0C
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Naf1 thanks for that article! There are indeed lots of worries about using acetone if one plans to store the acetone with HCl in it for any length of time, that idea alone makes me want to stray away from gassing in acetone altogether. My main worry is MDMA HCl and MDA HCl's slightly higher solubility in IPA than acetone. does anyone have the dielectric constant of acetone and IPA at 0C and 25C for comparison? these numbers below are the closest i could find:
taken from here h**p://clippercontrols.com/pages/dielectric-values
Acetone (77° F) 20.7
Acetone (127° F) 17.7
Acetone (32° F) 1.0159
Iso-Propyl Alcohol (68° F) 18.3
Toluene (68° F) 2.4
Xylene (68° F) 2.4
so combine your freebase with 4x v/v dry, freezer cold IPA and gas away. the freezer cold IPA will ensure HCl having a higher solubility in the IPA. BTW the 4:1 IPA to freebase volumetric ratio was pulled out of my ass, it just sounds like a roundabout nice volumetric ratio to use and is not based on HCl(g)/IPA solubility vs stoichiometric HCl to freebase amount like it should be based on. i must admit it would be really nice to find out HCl's solubility in subzero temp IPA so one could prepare a pregassed IPA solution, store in the freezer then add the right volume of it to your freebase (in excess of course).