posted 09-03-99 01:31 AM         

I am fairly familiar(sp?) with the making the HCl salt as I'm sure most everyone here is, but have there been any recent improvments or new methods? What I am proposing is basically a who's who of crystalization(sp?) techniques or something similar on the subject. I do remember seeing an FAQ around somewhere, but if I remember correctly it only listed a few different ways to get the HCl and no other options. I know there are other options available like Oxalic acid, Citric acid, Sulfuric acid. What would happen if one had freebase in DCM and added some GAA???

posted 09-07-99 12:20 AM         

Xtals for the teeny weenie batch

after A/B's, final extraction from based acid is made with small amt. of DCM, til aq. is clear.
the combined extracts are stripped of 'most' of the DCM. Toluene added to cover the residue and dissolve it. heat briefly (last of DCM) then cool in ice bath.

** heres the 'cool' part!

to the small amount of freebase/toluene in the 50 ml. beaker (teeny weenie remember) add 2 or 3 drops of water, and 1 or 2 drops of Bromothymol Blue pH indicator for aquariums. The indicator will find the drops of water and form a dark layer (blue) on the bottom. stirring with a glass rod will confirm this.
now add muriatic acid with an eyedropper one drop at a time, swirling or stirring with each addition watching the color of the indicator in the aq. layer.
each drop will 'discolor' the dark blue to yellow and swirling will expose new base to the indicator restoring the blue (dark) color.
eventually the dark will take longer to fully return or will not return. try to gauge it to one drop of acid and it almost stays yellow, or ideally green (hard to gauge.
by now, most of the color will have migrated from the toluene layer to the lower layer.

The rest of this follows Sunlights method basically, boiling and stirring, and adding more toluene if necessary to remove the last of the water.

watch the heat at the end.. it get hot fast.
remove from heat, cool in an ice bath.
cover the brown mobile oil (not the company you moron) with an equal sized layer of cold dry IPA. stir the mixture. add a similar amt. of EtO2 stir.
Xtals occur quickly in a purpleish mush (BTB indicator). filter, wash several times w/ cold dry acetone and proceed with snowwhite and the seven short dyklexuc kabalists.

dpHarma
over and out

posted 09-07-99 02:36 AM         

100 ml freebase mixed with
200 ml >99% isopropanol,

added conc. HCl (smoking) until universal
pH goes yellow-green. Cooled down.

Tip. Acid mixed with mag. stirrer (running all time).

Added min. 500 ml ether (anhydr.). Crystallization begin immediately.

Yield <= 80g (freebase contains impurities).

posted 09-07-99 12:03 PM         

dissolve base oil in 4X acetone which has been DRIED over MgSO4 and kept in freezer till 0C. Place this in cold bath (BEST-use dry ice in acetone, just a little) cool to less than 0C. 10C is ok, but more crystals will stay in sol.

While stirring, gas in HCl gas with a poly tubing from a generator. The generator is simply a bottle containing HCl (conc) with some NaCl..H2SO4 is dripped in and the gas is piped into the COLD solution. after a few minutes the crystals will come out and soon the stirrer will stop working due to the mass of crystals. Keep gassing until pH is no longer alkaline. You CAN overgas, but this seems hard to do and you probably will stop too soon. Just filter and then test the filtrate pH. If still basic, cool and regas it some more to get the remainder out. After you are all done, the acetone filtrate and any washes can be allowed to evaparate for a couple of days and any remaining crystals will come out (so long as you don't introduce any water in your washes)

posted 09-09-99 01:50 AM         

Make 10% sulfuric acid soln with dry EtOH (Or dry denatured alcohol, dry with molecular seives, CaCl or whatever) Dissolve freebase in dry EtOH (or as aid above) and add sulfuric acid soln dropwise and crystals form immediately with every drop. You'll probably have to filter a couple times to clear up the soln. Keep checking with pH paper and make sure it doesn't go acidic or crystals will dissolve. The elves on this side of town have only tried with MDA from NaCNBH3 and got snow white crystals. Need to take a little more because of molecular weight but a #3 gel-cap will blow your MIND. Any input for MDMA???

This is all for educational purposes only!!

the alchemist

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