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Purification of Mescaline HCl Options
 
An1cca
#21 Posted : 11/3/2017 5:34:33 PM

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Sounds great Endlessness. I already liked the method for precipitating spice-fumarate. Let it snow, let it snow...Big grin I will certainly give it a try while processing the following batch (that grows ever so slow Razz ).

Thanks again Biawak and Endlessness!
 

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Elrik
#22 Posted : 11/3/2017 9:36:18 PM

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In regards to post #1, I noticed that only the IPA was specified as cold. Was the acetone washing done at room temperature?

As a side note, after manually stirring the alkaloid with anhydrous acetone for a minute and only seeing it pick up a little color I dropped in a magnetic stir bar, covered the beaker with aluminum foil, and vigorously stirred it for 30 minutes. Boy was that more effective Laughing
 
An1cca
#23 Posted : 11/4/2017 6:39:29 AM

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Elrik wrote:

As a side note, after manually stirring the alkaloid with anhydrous acetone for a minute and only seeing it pick up a little color I dropped in a magnetic stir bar, covered the beaker with aluminum foil, and vigorously stirred it for 30 minutes. Boy was that more effective Laughing


True, I use mortar and pestle for this and only a minimal amount of acetone. Then I remove the solvent by sucking it up with a syringe through a small compressed cotton ball. After a second time, recrystallization solvent is added and the small cotton ball is squeezed dry.

After evaporation, the washing liquid dries to a black oil/tar. I can not imagine this stuff containing any appreciable amount of M. However, a clean run with 99% M-SO4 gave a loss of about 10% after three such washings Sad. Bad technique? Existent solubility?
 
DrSeltsam
#24 Posted : 11/5/2017 12:39:08 PM

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Elrik wrote:
In regards to post #1, I noticed that only the IPA was specified as cold. Was the acetone washing done at room temperature?

As a side note, after manually stirring the alkaloid with anhydrous acetone for a minute and only seeing it pick up a little color I dropped in a magnetic stir bar, covered the beaker with aluminum foil, and vigorously stirred it for 30 minutes. Boy was that more effective Laughing


Ad. acetone temperature: I used acetone at room temperature as the solubility of Mescaline HCl in acetone is so low. I think the most important factor is to make sure that the extract and the solvents are dry. Even at higher temperatures mescaline HCl will not go into solution with acetone - I tried recrystallizing from it and didn't manage.

The magnetic stirrer is a cool idea. I like that! Sadly I don't have one but if I were to have one, I would follow your advice.

An1cca wrote:

After evaporation, the washing liquid dries to a black oil/tar. I can not imagine this stuff containing any appreciable amount of M.


Hard to say. I would guess that it could contain up to 50% M. The impurities just need to be enough from preventing crystallisation. Btw. do we have any idea what this amber/black stuff is?
 
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