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Do the alkaloids usually crash out this fast? Options
 
mdtraveler
#1 Posted : 12/21/2015 5:32:46 PM

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120g powdered ACRB was heated in in approximately 500ml of vinegar. The acidic solution was vacuum filtered, and the bark was again heated in 500ml of vinegar and filtered. The solution was basified and extracted 3 times with cold toluene.
The toluene pulls were then extracted with 300ml of vinegar with a few drops of hcl to get the pH down around 3. The aqueous solution was then basified and extracted with 3 50ml volumes of hot naptha. Precipitates formed very quickly in the hot naptha, even as I was trying to remove the naptha from the separation vessel.
I was just wondering if it was normal for the alkaloids to precipitate this fast. The photo below was taken less than 10 minutes after the hot naptha was pulled from the second A/B and placed into the jar.
mdtraveler attached the following image(s):
tmp_18080-20151221_012400-240x427-732475569.jpg (26kb) downloaded 78 time(s).
 

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BongWizard
#2 Posted : 12/22/2015 10:07:44 AM

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Yes, this is absolutely normal. As soon as your solvent begins to cool, alks will begin to crash out and will result in the solvent appearing cloudy.
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downwardsfromzero
#3 Posted : 12/22/2015 10:46:56 AM

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If your solution is sufficiently saturated, they'll start to precipitate pretty much instantaneously on cooling.

Looking good!




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mdtraveler
#4 Posted : 12/25/2015 5:59:34 PM

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Thanks for the replies. Things did turn out pretty decent I guess. The results were mostly in the semi-liquid goo form, so no real way to get an accurate measurement for yield. The goo is pretty potent, as advertised, so I'm OK with it. Even the freeze precipitate stuff turned to goo despite doing the defats and carbonate washes and everything else. But again, I'm OK with that. Especially after the total fail on the bark from the first supplier. Thanks for all the assistance.
 
 
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