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a/b extraction of amides

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mtlmike68

Rising Star
Is it possible to make pure crystals of LSA? I've seen many a/b procedures for extracting from seeds but I don't know if these actually work. Using NaOH or HCl is supposed to hyrdrolyze the amide to a carboxylic acid, thus removing the nitrogen. This I think converts Lysergic Acid Amide to the two isomers of Lysergic Acid.

So how would could one get nearly pure LSA? The polar solvent method is very very crude. How could one recrystallize without damaging the goods? Is chromatography the only way?
 
piracetam here..

ideally, you'd want to evap a low-boiling crystallization solvent, like methanol or ethyl acetate, under vacuum. keep exposure to air and light to a minimum. If you want pure LSA (no iso-LSA), you'll want to elute it through a column of silica using ethyl-acetate:methanol: dilute ammonia, 4:3:1, using a blacklight to monitor the bands. LSA appears
teal under blacklight.

remember to keep the pH below 9, or there's a good chance it will all go iso.
 
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