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Anhydrous HCl in IPA preparation idea

Started by Bandil, June 02, 2004, 01:36:00 PM

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hest

100mL THF and 50mL HCl was mixed (exoterm) for 1 min, then 50-70g MgSO4 was added (more exoterm), and the mixture filtered.
Titration of the THF indikated an 2.4M HCl in THF solution.
Iff you don't have a fumehood cool with ice :-)
Ill give ether a shot later on.

Bandil

Kisses for you Hest  8)

Seems like a very easy procedure. Do you know how much HCl ether can hold?

Regards
Bandil


hest

When I gass ether I'll usual end up with an 5-6M so Iguess that's the limit.

hest

100mL diethylether was stirred with 50mL 12MHCl (exoterm) for 1 min, the ether was seprated from the HCl(aq), dryed with Mgso4. The MgSO4 was filtereed off and 10 mL of the ether was mixed with wather and titrated. yeald was an 0,22M HCl in ether solution.
Guess this could bee repeated to increase the ether-consentration (cooling and longer reacton-time might help too)

Nicodem

Adding some anhydrous CaCl2 into the HCl(aq)/Ether mixture would force much more HCl into the ether phase. Considerably more as the water phase would get way oversaturated with HCl. Don't exagerate on the amount of CaCl2 though, or you will gas the whole lab with HCl fumes. Just a sugestion to improve the otherwise nice and practical idea. :)


hest

The ether from the post above was treated with 12M HCl for 12H, seperated, dryet and titrated, still 0.22M.
So if we have 15g(71mmol) mescaline disolved into 100mL ether we have to add 322mL 0,22M hcl in ether to make the hydrochloride. Thats not good enough.