The Vespiary

The Hive => Methods Discourse => Topic started by: wacko_reaco on March 09, 2002, 10:13:00 AM

Title: HCl salt formation
Post by: wacko_reaco on March 09, 2002, 10:13:00 AM
if someone had a solution of MDMA in toluene and wanted to form the HCl salt without gassing could it simply be extracted into an excess of dilute HCl soution and the water and excess acid dehydrated off. I assume the answer is yes but the parameters that would be important are
-acid strength
-solubitlity of the salt in water so as to calculate the minimum extraction water required
-thermal degredation point of the solid salt so as not to overheat during dehydration of the solution
If anyone has any of these answers, or knows of any real life experiences please post
ta caio

wacka wacka wacka
Title: Re: HCl salt formation
Post by: blaztoff on March 09, 2002, 10:48:00 AM
Yes that would work. Thats the old school way. UTSFE [No 221244]
Title: Re: HCl salt formation
Post by: hest on March 09, 2002, 12:55:00 PM
Don't bee so lasy, dry the solvent, then gass (HCl(aq)+H2SO4) until pH is bet. 2-6 (weth pH paper)Much cleaner product. Gassing is the only way.
Title: Re: HCl salt formation
Post by: PurpleSmurf on March 09, 2002, 04:37:00 PM
Is there any way to fix overgassing?  SWIM dried the toluene with (supposed) product and gassed.  The solution went from a colorless solution to light pink, with no crystal formation.  Is this run wasted?  Is there anything to try to get crystals from this?
Title: Re: HCl salt formation
Post by: hest on March 09, 2002, 05:26:00 PM
A/B wash the solution.
Then yoy v'can use HCl disolved in methano;ethanol;ether... and drip the HCl solution into the toluene, thig give you much more control over the gass.