calcium chloride contamination (D*mp R*d)

[hexagonium]

Rid me of this dam(p) rid. Swim attempted to recrystallize his beautiful end product using the dual solvent technique(ala Geezmeister). By mistake, swim had dried his alky with calcium chloride instead of baked epsom. He went about the recrystalization process and at titration,  was left with meth and a gooey substance that would not dry. Then he inexplicably added water to the mess to see what the stuff would do. Now, he has a beaker-full of h2o, CaCl goo, and meth. 

Since this is a good amount of end product, Swim needs some guidance in cleaning it up.

Please keep it simple for this simpleton? Thanks.

[Relux]

[autumn_lamb]

and so would be interested in some additional replies. she likes relux' 1st option:

In that case, you could dissolve your product in hot ipa (you cannot use another alcohol because methanol will dissolve CaCl2 and ethanol will not let go of water (which would dissolve CaCl2). Anyway, when your product is dissolved in IPA dry the solution with your epsom. At least now you will have a calcium chloride-free and H2O free solution of the product. Unfortunately you will still have whatever your bunk CaCl2 left in there.
  At this point you could reduce the volume by evaporation until highly saturated and then flash out with acetone or favorite NP. Then you would have cleanish crystals that you could try and recrystallize once more. In fact, at this point you could probably come up with some way to continue into the recrystallization that you planned on in the first place, instead of crashing it out.

because she only titrates and does not gas. would following relux' suggestion cited above result in somewhat clean meth?

[Relux]

If I have information that is mis-information, by all means list it as mis-informative, but you should at least either say which part of that information is bad or offer some good information instead. Then I could learn something too, maybe.

Crap. I was pompous enought to think I could avoid bad karma.

[lugh]

Unfortunately, solutions to complex problems require knowledge of the matter at hand, not useless simplifications    An old saying of great worth states that those who don't bother to learn the mistakes of the past are doomed to repeat them    For example, see

Post 284140 (missing)

(MustaphaMond: "Major CaCl2 infection", Stimulants)    Here are the applicable sections from Avery Morton's Laboratory Technique in Organic Chemistry:







Note that Morton states this to be a recurring mistake made by those learning organic chemistry. Recovering the amine product from the amine/calcium choride addtion product requires dissociation of the complex salt using heat and pressure, here's the abstract of the paper that would need to bee retrieved and translated to provide enough clues as to a workable recovery procedure:

[autumn_lamb]

sounds as if hex's go should be trashed unless he's astute in chemistry. not even an a/b is worth a try?

[Relux]

[Relux]

[Organikum]

Nevertheless, I remember that FMan in his earlier days used the CaCl2 addition product for recovering the amine from the reaction, I dont remember though how he decomposed it lateron.

A search for FMans old posts might be helpful.

[Osmium]

FMAN also reccommended lead metal as a hydrogenation catalyst. He didn't make much sense most of the time.