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Topic: Purification of Hydrochloride  (Read 1633 times)

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Offline Moi

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Purification of Hydrochloride
« on: April 30, 2015, 04:45:11 AM »
Hi all.

I have a question about which is the best way to purify an amine hydrochloride from inorganic salts. The trouble is that to prepare that hydrochloride I could not use a solution of HCl in ether or THF, and I dissolved my free base amine in THF and added an excess of aqueous HCl, so now I have my hydrochloride in a mixture of THF/water and NaCl in solution.
What do you think is the best straightforward way to eliminate the inorganic salts (NaCl) and obtain my pure hydrochloride. I would eliminate all the solvent under vacuum and do reverse phase chromatography, but in my lab I don't have the possibility to do a RPC.

Thanks,

Offline Hunter2

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Re: Purification of Hydrochloride
« Reply #1 on: April 30, 2015, 05:13:35 AM »
Where is the sodium comes from. You add your amine and hydrochloride you mentioned.

Offline pgk

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Re: Purification of Hydrochloride
« Reply #2 on: April 30, 2015, 11:29:11 AM »
Recuperation of the free base:
Neutralization → solvent evaporation → extraction in dichlomethane → removing of the aqueous phase → drying with Na2SO4 → dichloromethane evaporation.
Salt formation:
Solution in an oxygen containing solvent (e.g. THF, ethanol , isopropanol, etc.) → saturation with gaseous HCl at oC, (ice bath ) up to acidic to litmus (open flask in the fume cupboard) → cupping and storing in the refrigerator, overnight → filtration.
If not equipped, try an organic acid.
But, where is the sodium comes from?

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