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Crystallisation questions

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XrLeap:
Hi,

SWIM has been using this method to make salt:
Post 107417 (missing) (Osmium: "Re: MDMA HCL/MDMA sulphate -> ?", Methods Discourse)
It is wonderful that when the IPA solution is added to ther ether, salt forms. What has the water from HCL become now? Does distilling the ether solution to obtain ether reuseable? SWIM tried but the distilled ether could not form salt the second time. What can be done to make it re-cycleable?:)

XrLeap:
SWIM is thinking using 3A mol sieves to remove H20 in the IPA solution before forming salts in cold ether, will this be ok?:) This will help to reduce the amount of ether used(20 times the volume of amine).

indole_amine:
The sieves consist of Ca or Mg ions (don't know exactly), and therefore are ACID-SENSITIVE! You cannot make anhydrous IPA/HCl or IPA/H2SO4 with it, it's gonna partially dissolve and give Ca/Mg salt contamination...

Better try dissolving your freebase and the appropriate amount of aequous acid (HCl 37%? Because H2SO4 can be had in 99% conc., no water present, no drying needed.. 8) ) in toluene, remove water by distillation using a dean-stark separator (or simple still setup, and returning the non-aequous layer to the dist. flask continuously), and cover the remaining yellow/range melt with at least 5x its own volume of anhydrous, cold 9:1 ether/acetone mixture and let sit in freezer for one day. Sparkling little beauties (that is, if you used HCl - sulfate hardly gives crystals).

Enjoy.

indole_amine

XrLeap:
Thanks, [/b]indole_amine,

for the reply.

The sieves consist of Ca or Mg ions (don't know exactly), and therefore are ACID-SENSITIVE!
--- End quote ---


so, can SWIM use 3A mol sieves when the pH is above 7? When pH is above 7, the acid could have all reacted with the amine right, leaving no acid behind. Is this logic correct?

Meaning, when HCL or other acid is added till pH 8, SWIM would stir the hell out of it and then add the mol sieves to absorb the H2O under non-acidic condition. After stirring for a while, then filter the mol sieves away. Is this method ok?:)

indole_amine:
Buffering the acid with amine freebase, so it can't hurt the sieves... so to say.

Yes, it should work, if you UTFSE for Bandils posts you will find exactly such a crystallization method... ;)


indole_amine

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